# 2 Layers after precipitation, what is causing separation?



## Alentia (Oct 15, 2011)

After making my test run with 0.6 gr of 10K+ 0.1g of 18K gold and getting 0.32g of gold powder I have decided to run another test with 62 gram of 10K gold scrap.

1. I have reduced copper and silver by HNO3/H2O to the total of 38.79gr or 62.67% of total weight. Estimated net gold should be 62*417=25.85gr. Meaning I still had about 13gr of Cu and Ag, which would not dissolve.
2. Made 5 portions of AR (about 65ml +15 ml H2O or 80ml total)
3. Run 5 portions one at a time (one after another). Then combined all 5 solutions together.
4. Evaporated whole solution using H2SO4 and HCl
5. Added drop (literally) of Urea (no fizzling)
6. Diluted with 3-4 parts of distilled water and filtered. My solution is green/yellow I guess due to excess of copper.
7. Added SMB (not diluted in water), no fizzling. Gold started to drop slowly.
8. Got precipitated gold at the bottom


I have 2 questions:

1. Why am I getting 2 layers of liquid? One is yellowish at the bottom and second is above - teal (with copper) with separating ring, which looks like AgCl or something else floating in between layers?
2. During 5 staged AR additions, I used temporary container - volumetric flask. I have gold residue on inside walls. How do I get it out? Shaking with AR?

I have encountered another issue:

On my 5th run with AR, very little gold was remaining, My pyrex beaker cracked on me and all solution went into my sand bath. (I did not add this solution to my main solution)

1. I have picked sand, dropped it in AR, added water and boiled for few hours
2. Filtered
3. Added water and reboil
4. When I dropped bit of H2SO4, white stuff started to form and after adding little bit of HCL it looks like gelatinous chloride.
5. Added hot water. I have separate a bit of liquid from main beaker and tested. Liquid tests negative for gold with Stannous. SMB simply dissolves in the liquid nothing drops. I am guessing there is gotta be something in that white gelatinous mass.

I understand I got some kind of reaction with Si Au and AR and whatever salts were in the sand. Sand was from Dominican beach. I doubt there was Pb in the sand. What did I get? There might very well be about 0.2-0.5gr of gold. Is there a way to break that gelatinous stuff or it is not worth it? This is more for the discovery and interest.


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## butcher (Oct 15, 2011)

I am not sure this will give answers, but here is what I think.
I believe the sand would have base metals (like Iron) that could cement your gold out of solution, and these would need to be removed to get the gold, I would incinerate the sand as they may also contain sulfides or other mineral/metal salts, and leach base metals before trying to extract the gold (if there was enough gold in this to make it worth the cost and trouble).

Some times you will get layers in chemical reaction for several reasons, like dirt, oil, or organics in solution, reactions not completed, not enough reagents, or even too much reagents, other reactions in metal solutions like a base metal in a gold solution, or even metals like tin that will not completely dissolve but will jell up, colloids in solution.

I would try a strong heating and make sure acid content was high and then see what happens.


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## Alentia (Oct 15, 2011)

Thank you, Butcher!



butcher said:


> I am not sure this will give answers, but here is what I think.
> I believe the sand would have base metals (like Iron) that could cement your gold out of solution, and these would need to be removed to get the gold, I would incinerate the sand as they may also contain sulfides or other mineral/metal salts, and leach base metals before trying to extract the gold (if there was enough gold in this to make it worth the cost and trouble).



There is no more sand, it is the "white jelly" and liquid with no gold in it. Is there anything in the "jelly"? and what exactly can I do with it?




butcher said:


> I would try a strong heating and make sure acid content was high and then see what happens.



You mean HCl, correct? You mean boil the solution with dropped gold inside or filter first and then boil?


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## butcher (Oct 15, 2011)

??? Are you saying you completely dissolved the sand into that white gel???
What and were did this sand come from?

Well sand usually has a high percentage of (quartz) silica (what they make glass from) and that usually will not dissolve in the solutions we are discussing, sand is also small rock or ore, I suspect your sand is not what I think of as sand. if there was gold in it then there still should be gold in it, if the solution tests negative (a negative test can be for several reasons), if you have nitric acid (or other oxidizer) in your solution you are testing for gold, you will not get a positive reaction as any gold that was trying to react with the stannous chloride to turn colors would just re- dissolve and give you a false negative reading of your test, or another reason for negative test could be your testing solution is not working (test your test solution with a known gold solution) and then a negative can mean there is no gold in solution. In that case it should be in salt form, (usually as black or brown powders).

Cementing with copper buss bar if gold is dissolved in solution,
Or if in powders try and get it into solution if possible then separate it from the junk that will not dissolve then cement gold back out of solution onto copper.

I was talking about colloids in solutions (they are like two electrons neither negative or positive fighting each other and holding each other in suspension)
Heat and high acid content sometimes helps to break colloids< I am not positive that is what you have but it is worth trying until someone else give you better clues, boiling is not necessary just heat below boil for a while this will also concentrate solution raising acid concentration, I would probably add some HCL also.

http://mysite.du.edu/~jcalvert/phys/colloid.htm

http://en.wikipedia.org/wiki/Colloid


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## Geo (Oct 15, 2011)

what material did you start with? was it E-scrap or black sands concentrates? if it was E-scrap the white "sands" could be tin (II) chloride which you have turned into metastannic acid.that could be the white gel. at least that's what it looks like as for the separation someone else will have to comment on that.


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## Alentia (Oct 15, 2011)

It was just regular 10K gold scrap jewelry.

After vigorously stirring the solution the layer is gone. It looks like the separation was made of trapped bubbles of SO2.


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## dtectr (Oct 16, 2011)

Just my random dos centavos - 
_Beach _sand (from Dominican Republic or Dominica?) would of course be contaminated with sodium chloride, also possibly iodine from seaweed (kelp), both solvents for gold, under the right conditions. I doubt if either would survive the extensive processing, though?
Coral sand and/or sea-shell sand would be calcium-(what? carbonate? anybody?)

I was going to suggest, though it seems you figured it out, That a concentrated dirty, solution could create layers of varying densities. lazersteve recommends diluting auric chloride by double, up to quadruple; he suggests it primarily for forcing silver chloride out of solution prior to filtering, then precipitation.

NOTE: I hope this (following) isn't viewed as a hijack - the images illustrate my thoughts, and i believe it to be relevant:

I've postulated on this before, Hoke stated that sulfur dioxide (produced by reaction from SMB) is best used on neutral, or slightly acidic solutions. The common practices used by many members, i.e. super-dilution, packing with ice, etc. - wouldn't they serve to raise the Ph to nearer neutral, making sulfur dioxide more effective? Wouldn't it also lower the risk of drag-down?

Forgive my ramblings - I've caught my annual virus and feel like, well, you know. I'm gonna take my meds & go back to bed.

keep us posted & good luck <<groan>>
edit: typos


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## samuel-a (Oct 16, 2011)

Looks like Orthosilicic acid or some other member of the Silicic family.. :mrgreen: 

but that's just a shot in the dark...


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## Alentia (Oct 16, 2011)

Now I have hit another interesting issue.

After precipitating gold from the solution, the solution came out to be very clear light green color.

1. I have added too much SMB as solution have strong smell of sulfur when siphoned to another vessel
2. Solution was sitting with SMB for 48 hours and I should assume 99.9% of gold has precipitated
3. Test with 3 days fresh stannous is negative (keeping it in dark glass bottle) actually resulting in "yellow" color, which I should attribute to "iron", if correct.

Now, when I add "Salt"not ionized to the solution I do not have AgCl dropping down. Salt got dissolved and that's it. As per previous calculations I suppose to have at least 13gr of contaminants: silver, iron and copper. Based, that my solution is green, looks like majority of it is iron. It is possible to think that solution is green because of "yellow Gold" and "Blue Copper", but as it was with SMB for 48 hours, gold is precipitated. But, I might be totally wrong!

What is causing AgCl not to drop, other then absence of it in the solution. Could it be that too much SMB won't let AgCl precipitate?


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## butcher (Oct 16, 2011)

Silver or AgCl is insoluble in these acids, (so basically it will not be in aqua regia).

Very little silver can form AgCl2 this little bit of silver salt may carry through your process until you dilute the acid, at that time it becomes AgCl and precipitates as white silver chloride salt.

You may not have had much silver in solution.

Too much SMB and other metal contaminates could give a yellow solution (I think Iron?).

I believe the silver would precipitate even if you had an excess SMB, and even could form silver sulfate depending on how much excess we are talking.

It seems you may have some base metal contamination and an excess of reagents.
Very good post dtectr, very good thinking on that sand (I guess I just think of river sands), one point I would like to make, adding water (dilution) will not change PH, that is a function of (adding) acid or basic solutions, water is neutral, so it just gives the acid or base ions more room to move around.

Percentage of hydrogen is PH, in water the Hydrogen and oxygen are bonded very strong (if that’s what they call it). water can be separated with electrolysis into hydrogen and hydroxides, but normally will not separate.


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## Alentia (Oct 16, 2011)

Thank you, Butcher for enlightening! What am I thinking... I have already deposited all AgCl into my AgCl container from AR. I guess I am left now with Cu and Fe in the solution and whatever else might have been there like Zn, Pb and Sn. Solution is emerald color.

On another thought about sand boiling in AR. Could it be that gold got precipitated by the sand and now is in the sand, when beaker cracked? The white stuff I got is possibly by product of sand salts and gold precipitation... could it be? Can sea sand precipitate gold?


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## butcher (Oct 17, 2011)

I do not know about the ore in sand in your beach, but sand around here can contain metals, metals can precipitate gold from solutions, also the ore may contain other anions (like sulfates) this could make an iron sulfate and precipitate gold, sand or ore can be very complex mixes of anions and cat ions, some like manganese dioxide in ore if mixed with HCl will even dissolve gold, where HCl alone will not.


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## qst42know (Oct 17, 2011)

Sands from a salt water beach are likely to have coral and shell origins and as such big consumers of acids. 

What is the PH of your solution?


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## Alentia (Oct 17, 2011)

I do not have litmus paper to identify solution PH, but it looks like alkaline at or above 7. Sodium Hydroxide is not causing any immediate reaction. Looks like that "white stuff" consumed all the acid. The sand is full of organic matter like microscopical pieces of shells, etc.

I have strong feeling that my gold has precipitate into the sand in tiny particles. Are there any known method to get it out of there?


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## Alentia (Oct 17, 2011)

After all I got 25.11 gram of gold powder, which I assume should be 99.8-9% pure. This falls short of initial estimate of 25.73 by 0.62 grams. I am guessing my calculations of loosing about 0.3-0.5 gr in the sand is correct. The rest is attributed to ~ gold content in 10K jewelry. So the question remains, how do I recover gold from sand I have used for sand bath.

Will use water bath next time...


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## Harold_V (Oct 18, 2011)

Alentia said:


> So the question remains, how do I recover gold from sand I have used for sand bath.


I'd suggest a start with nothing more than a water rinse. If the resulting water tests negative, it's likely the gold has cemented on something within the sand in question. You may or may not be able to make a recovery that is economical. You may be well served to consider this a part of your cost of learning and move on. My logic is that if the gold has cemented, you're likely to be troubled by the substance(s) that cemented the gold, which will make recovery difficult, if not impossible. 

In all my years of refining, I never used a water bath or a sand bath. I used thin asbestos gauze or sheets between my heat source and the beakers I used. When they became dysfunctional, they were sent to my waste materials for processing for traces of values, which are sure to be present, just as the sand you speak of. 

If you have plans for furnace work at some point in the future, you may wish to consider adding the sand, along with soda ash and borax, to a charge. The soda ash will dissolve the sand (assuming it's silica) and liberate the traces of values. If you have a collector present, you should recover the vast majority of the gold tied up in the sand. The negative here is the potential to include something that complicates processing of the recovered values, but that was never a problem for me. 

Harold


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## Dr. Poe (Oct 25, 2011)

Before I tell you what I think, let me tell you what I've had in the past. I had the very same accident with the same results. I dried the white flakes and cupelled them with lead. The product was 23+K gold. It turns out that boiling with H2SO4 to fumes produces SO2 gas which precipitates gold, but that wasn't why it happened. When H2SO4 is boiled with silica sand in the presence of sufficient water a substance is produced that is a hydrated silica oxide. This oxide hydrate is exactly the same formula as is oxallic acid except that silicon atoms substitute for the carbon atoms. The action on soluable gold salts is almost the same except SiO2 is formed and precipitated with the gold instead of CO2 gas. Often Leaching from sand with strong acids will dissolve some Silica as well. Hindsight is 20:20 but it's always better to check your glassware for cracks.


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## samuel-a (Oct 25, 2011)

samuel-a said:


> Looks like Orthosilicic acid or some other member of the Silicic family.. :mrgreen:
> 
> but that's just a shot in the dark...





Dr. Poe said:


> Before I tell you what I think, let me tell you what I've had in the past. I had the very same accident with the same results. I dried the white flakes and cupelled them with lead. The product was 23+K gold. It turns out that boiling with H2SO4 to fumes produces SO2 gas which precipitates gold, but that wasn't why it happened. When H2SO4 is boiled with silica sand in the presence of sufficient water a substance is produced that is a hydrated silica oxide. This oxide hydrate is exactly the same formula as is oxallic acid except that silicon atoms substitute for the carbon atoms. The action on soluable gold salts is almost the same except SiO2 is formed and precipitated with the gold instead of CO2 gas. Often Leaching from sand with strong acids will dissolve some Silica as well. Hindsight is 20:20 but it's always better to check your glassware for cracks.



Bullseye 8) :mrgreen:


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## core (Nov 4, 2013)

Wow! This is beginning to make more sense to me. I am working with an ore that has undergone these conditions naturally (I think). The veins from an oceanic plate convergence in the country rock are filled with what looks like beach sand at this particular formation. Hot concentrated sulfuric acid solution being shot into seawater of an ancient shallow sea. 

Ive been stumped as to why I can drop au from solution with smb or oxallic acid and everything goes as expected untill the wash cycles. Then a white powder appears. I can dry the powder and heat it slowly as it changes into the yellow, red, then brown au metal. Only upon melting it just wont stick together. You can see the characteristic green associated with gold mixed with glass. 

I can fuse it to lead, but it seems to be absorbed into the cupel and also certain melting dishes that Ive bought.

I think that im gaining on it though, having cemented with copper and am trying to refine the powders. I have determined that tin is present as well as chromium causing me hassle. I have DMG on order and is due in any day so I should be able to determine nickel and palladium being present soon.

I have had two assays from seperate companies that both seem inaccurate to me; They don't resemble one another and show no preciouse metals from fire assay, ICP, or XRF. I dont really want to go into my experiences with assayers to much. I may have ordered the wrong type of test for my materials this last time, but neither time were the folks very helpful even though I tried to explain. Im not laying blame, I just want a good job. This is complex and mistakes do happen. 

Upon cementation with copper tubing- I see a couple of different shades of silver. A third shiny one (hg) and then gold will cover that. There are definately values present. 

Throughout these bench tests that I have done, I tried incorporating activated carbon to catch colloidial gold solutions. I also experimented using it as the cathode in a cell. Last night I incinerated all of it and chose to begin new process with a fairly concentrated- hot naoh boil in an iron skillet to eliminate carbons and chromium first. The results of that production was blood red salt water, and the same for a second clean water rinse. 

So, I think It is leaching the Au from the mix which would be great providing I can find a way to recover it. I seem to recall reading somewhere here how to break the colloidial solution of au in naoh, but I cant find it again. Can someone help me out with this? 

And also Could you elaborate more on the reaction of Au being precipitated by siO2? How or what can I do with this? The AU will go into solution with just hcl and after a time and the reaction slows and a small nip of bleach is added.

Ive decided to have one more assay performed and have been referred to a reputable firm. What is the most sure way for me to pre process this material and what type of assay should I order? I was thinking of sending just the cemented values from the stock pot. Im not sure what to classify this ore as- an Oxylate? Chlorite-ate? Sulfide refractory or double refractory? I would like to know the base metals present as well. A four acid assay perhaps?

Im really thankful to you all for the posts from the past, present, and future. Im learning new fascinating things here everytime i log in, and have come a long way from where I began almost a year ago. Thank You for your patients and attention.

Core


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## butcher (Nov 4, 2013)

core,
It sounds like you are trying to leach an ore.
Ore can be a wide variety of metals, and can be sulfides,oxide or a number of other an anion, basically rock can be a complex mix, and there are many different mixes to make up different types of rock.
leaching may not always prove successful, and in fact many times you could end up spending a lot of time, money and acids leaching just the base metals from the ore and not touching the values, also to leach the gold or even the base metals many times you would have to put them into a state that the acid would dissolve them, sometimes roasting will drive off sulfides (sometimes iron is needed in the roasting process, before the acid can attack the metals bound up as sulfides, sulfide ore is very common but it is not the only type of ore, halides, oxides, hydroxides, nitrates, sulfates, chromates, molybdates, tungstates, phosphates, arsenates, vanadates, silicates, and even organics, basically the ore can be compounds of very complicated chemistry, and so can the chemistry when trying to leach, the rock can change the chemistry of the acid, the metals in the ore can be in a state that the acid cannot dissolve, basically leaching may or may not work at all, and normally even if the acid leach will work the ore needs pretreatments to put it into a state that the acid can leach it.

Usually the ore will also need concentrating the values, before most any kind of extraction process is used (concentrating the more valuable metal, separating it from the bulk of the gangue ore).

Knowing the chemical make up of your ore would be important to help you determine a method for extracting values.

But most important would be a good assay to see if there was even enough value to try and recover, not an assay of concentrated material, but an assay of the whole mining area, so that you know how much values per ton, of the whole lot, not just sweet spot or of a good looking stone.
If you pick a stone that looked promising and sent it in for assay, say it had visible gold and got you exited to mine the area, now this assay of this stone shows high gold content (as it should you looked hard to find that one rock that would), but the most of your mining area is barren of gold, now your mining tons of rock spending money and getting nothing in return (all based on one good looking rock) the ore sample should be a wide mix of a Representative sample of the are your are planning on mining.

Working with ore and working with more pure metals in solution are completely different ball games.

You state your gold is will go into lead, but when you cupel the lead the gold goes into the cupel with the lead oxide (that is not gold, but an oxide).

you also mention your gold when melted will not stick together or You can see the characteristic green associated with gold mixed with glass. Again this does not sound like gold but an oxide.

Note working with Ore and acids can be dangerous, again knowing the chemistry of your ore can be important, you can easily gas yourself to death pouring acid onto an ore that was an arsenate compound of ore.

Also treating your waste solution and disposing of it properly and safely, without concentrating your values, you could use tons of acid to get a speck of gold and have tons of toxic waste on your hands.

If the gold was free gold mechanical means to get it would be my choice, if the gold is bound up in the ore, either mining and selling the rock or just forgetting it and moving on and finding a place I could mine free gold would be my next choice.

You are not likely to do much good leaching ore,


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## core (Nov 6, 2013)

Hey Butcher,

Thank you for posting your thoughts here. Ive read many, many of your posts and even have some printed out and useing as reference. I know that you know what you are talking about and appreciate the effort that you have put into considerately sharing your expertise with the less knowledgeable. Books can't replace the value of experience as a teacher- greater than the sum of both is having an experienced teacher.

Respectfully, I say that I think you must have me confused with some other incredibly strong and handsome prospector. I consider safety number one. I work under a fume hood, and use every precaution to protect this fine figure of man. I respect the law and consider myself an outstanding-upstanding citizen with love of god and country. I am not creating toxic waste and destroying mother earth-I just want to milk her teats. I treat my waste solutions exactly as recommended here on this forum, and have them printed up and hanging on the wall out in my work shop. No cause for alarm, but thanks for your concern.

In fact if I could find a way to be any "greener", I would take action because Im getting sick and tired of my neighbors calling me "white-boy" :-}

A few dumb and irresponsible prospectors have caused society to generalize the entire lot poorly. This is not me... Im not about to mortgage the farm for a gold bug epidemic while hollering "eureka" and acting like a madman. Im just an inquizative-honest, hard working country-boy with an appreciation for the outdoors and a fascination for the natural sciences and "inner workings" of things. 

I live in the here and now, being down to earth and rational most of the time. The FBI granted me clearance to work inside a nuclear generating station (of course I didn't mention my burning desire to be a dirt welder) so they consider me safe and sound. I must admit to you all though that I have come to blows defending the existence of Santa Clause, but that was way back when- on the playground as a kindergartener. So....I realize that it sounds too fantastic and unreal for someone other than a scientist to uncover something new especially in this age of information/technology. If the reader of this happen to be of the naysayer type, take the easy road, and think inside the box type then please excuse the notion and my quest for discovery,knowledge, and understanding by not posting words of discouragement.

I have a lot of "issues" to work out and processes to refine, but to pick just one to focus on, I need help with the melt. 

I have a million questions and am certain that Im fouling things up since Im learning from the experience of "on the job training" and the written word. Keeping that in mind while considering my observations and theories, correct me where im mistaken, please. Im open minded and can/am willing to follow instruction if you have any constructive courses of action to perform. 

In my research I have not heard of such a thing, but just suppose that au has been lode deposited from solution with silica in the crystal matrix as described by dr. poe. The lode ore at this spot looks like fine grained diatomaceous earth instead of say white milky quartz for example. I think it may have metamorphed from a the previous event of tectonic plate collisions during uplift and subduction. If the crystal lattice did contain silica and pm, base metals or combination thereof= what would the best process for recovery be? The very finely devided stuff im calling values seems to want to go into the slag instead of reduce into metal. I am thinking that I just have not allowed enough time during the melt and need to thin the slag more. Each time I melt the same slag it seems to reduce more. Lacking the experience for comparison makes it hard for me to decipher results.

On the same subject I ponder the discussion between yourself and dr. poe about incomplete precipitation and the gold carrying a plus one static charge. I have yet to digest the mechanics of all of that after reading through it again and again. Then again and again, but that is describing the results of my multiple attempts at reduction via oxallic acid or smb where everything goes as expected during the drop and looks right, but converts to white powder during the wash cycle.

I had stated that it would fuse to lead as a collector. To describe in more detail- I did not use any flux for this. Taking that bead through the rolling mill as thin as possible, I can see splotches of the same white powder and slightly different shades of color here and there. Could the white powder from the bead be a broken window so to speak where the silica had been linking atoms or molecules in the primary material? The white powder was not there before i introduced lead and the bead was clean. I suppose the lead could have easily encapsulated some of the gangue material and crushed it. I just wanted to mention this white powder showing up here as it rears itself at strange and unexpected places throughout the process. Im aware that lots of metal salts are white.

It is not practical to pan this vein material as it is all so finely divided. Ive tried screening to 100 mesh and very carefully concentrating it. Fine gold is present but the heaviest thing in the pan is white. I guess plattinum but the action of the particle is relative to its size and shape which is to small to determine. 

Having undergone multiple major geological events it seems possible. The area is documented to contain flour gold and there is a working hardrock gold mine twenty or thirty miles from this place. It is also known for some rare earth metals. A geological wonderland of granite, limestone, and precambrian host rocks with intrusions in each containing slightly different makeup... Cool stuff to rockhound like myself. Yes, There is some free gold that can be seen under a jewelers loupe in the deposits that resembles a picture of whitwatersrand surface ore. Out of three different lodes- One of these spots in this range has a round silica pebble agglomerate containing much cinnabar- Im shying away from this one even though it looks richer. Some of It looks like really fine clumps of freemilling gold to me. Some of it looks and behaves like gold having been dropped from solution and during the wash cycles for refinement.

This post is getting too long, so as to not talk your ear off or eyes out, I shall condense. 

I need more detailed instructions on the safety and process of alkyline leaching. Am I correct in my understanding that trends are moving away from cyanide for safety and environmental reasons? I have a pound of sodium thiosulfate on order to experiment leaching on the basic side. I read that cyandide leach is much more selective for gold but I cant seem to locate a supplier for that or detailed procedure.

Another area I need edge-u-macatin on and would like to explore further is froth flotation as a means of concentrating, but detailed information and instructions I have been unable to find.

Again, I say "thanks ya'll"

Core


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## g_axelsson (Nov 6, 2013)

Just a heads up on the so called "Dr Poe", he was eventually found out to be a lot of words and no substance. It seems he had read a lot of theory and by sounding advanced he managed to propose theories that wasn't true. In the end he was found out and banned.

This is why the footer of his posts should have a warning sign!

As for gold-silicate minerals... there are none known. http://athena.unige.ch/bin/minfind.cgi Look for Au in the chemical formula and you will find out the truth. Gold ores and their geochemistry has been researched so much that any new natural occurring mineral with gold and silicon would have been found by now.
Gold can be encapsulated by silicates and other minerals but if it is exposed it should be able to leach it.
http://www.sgs.com/~/media/Global/Documents/Technical%20Documents/SGS-MIN-Tech%20Pub-2004-03%20Process%20Mineralogy-LR-EN-11-09.pdf

Göran


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## butcher (Nov 6, 2013)

Froth floatation, a way to concentrate sulfide ore;
https://www.google.com/#q=Froth+flotation+of+sulfide+ores

https://www.google.com/search?q=Froth+flotation+of+sulfide+ores&source=lnms&tbm=isch&sa=X&ei=d3F6UtOGJujUiwL5_4HwAQ&ved=0CAcQ_AUoAQ&biw=939&bih=533

There is also some good information on the forum from some members who have used froth flotation to concentrate values from their ore.

Core, I didn't mean to put you into that little box, it is just we get so many people coming here who will dump acid into a complicated mix of ore creating dangerous gases, thinking they can leach gold from a bucket of unknown ore (they have no idea of its chemistry or the reactions they will be creating, or even how much if any gold that bucket may or may not contain) with a few gallons of acid, expecting to get rich, all the while putting themselves and others in danger.


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## niteliteone (Nov 7, 2013)

core said:


> Wow!
> (snip)
> I can fuse it to lead, but it seems to be absorbed into the cupel and also certain melting dishes that Ive bought.
> 
> ...


These 2 statements should tell you more about what You don't have than any other. (A viable product)



> (snip)
> I have had two assays from separate companies that both seem inaccurate to me; They don't resemble one another and show no precious metals from fire assay, ICP, or XRF. I don't really want to go into my experiences with assayers to much. I may have ordered the wrong type of test for my materials this last time, but neither time were the folks very helpful even though I tried to explain. I'm not laying blame, I just want a good job. This is complex and mistakes do happen.
> 
> Upon cementation with copper tubing- I see a couple of different shades of silver. A third shiny one (hg) and then gold will cover that. *There are definitely values present*.


You have listed the 3 most used assay methods available to prove PM's, But yet you insist they are wrong and you have gold, silver and PGM's in this material :shock: 

May I suggest you bring in an uninterested 3rd party to collect the samples and handle the testing, as the haze of this war might be affecting your better judgement.

I say this in a good way with no ill intentions


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## core (Nov 7, 2013)

Thanks guys,

I mis stated the cupelling part. I was trying to use a new cupel as a melting dish. Using a torch since I burned out the elements in my el'cheepo gold melting furnace just isn't cutting it. Ive come to realize how important a controlled temperature is. I could not bake a cake with a torch, either.

I think a lot of my problems i described have been caused by si and carbon being in solution. I had learned that they needed to be eliminated A long time ago but just plain forgot until I read this post. What actually happens in the reaction with them present? Just curious. 

I asked about the best assay... My first tests were by the procedures you prescribe, Butcher (roasting first) then a water boil rinse. Having altered the sequence of acids and rinses applied I decided to try variations on the raw material to observe the effects. The complex has sulfer and chlorine elements. If I use sulfuric acid as a first step pretreatment then I can smell chlorine being released. If I take values straight into a hcl/cl or AR solution and cement with copper after a few days the copper quits doing much. So I introduced a piece of zinc sheetmetal to stir with breaking the chlorine complex which evolves the smell of sulfur. What would I classify this ore as? I want to not waste any more money on an assay, but don't mind paying more for a chemical analysis if necessary. I don't think a basic fire assay will work with the ore since the au is an oxide or in complex matrix. With the temperature of either oxygen or chlorine expelling so go much values-Ive noticed from the smoke and cleaning the fume hood filters.

What do I classify this ore as? What types of assays should I order? 

I am correct- without a doubt- of values being present if they will cement out onto copper, right? Not saying how much of which metal, but definately present- wouldn't you all agree? Another fact that I failed to mention is that the melting temperature of the metals parted with nitric from a lead fusion was higher than 1150 C. My graphite crucible did not like these charges and broke when I was stirring. The graphite cruscible would also have black fuzzy metallics stuck to the outside of it after a charge (sounds crazy- I know)_ I had to add lead back into the charge to get the cruscible cleaned out. My new furnace will be here in a few days along with some dmg+ from pics and info found here evidence points toward palladium and in higher quantity than au.

I will continue to study, I could certainly use more of that. I wish I could find an online class/course that would teach this stuff. Im not looking for a degree program just a disciplined course of study with a teacher. Some of you folks here ought to get together and offer something like this. There are so many different specialties and processes in refining and to add working with unknown substances makes it more difficult. I find myself skipping around alot and by time I find what im looking for Ive already found two more to look into:> Having a teacher to argue with and answer to would help me to focus. I have no idea what a mining consultant charges, but I imagine alot. I have Ammens book, and It is a pretty darn good overview of many aspects, written in a way that i can understand, but not real detailed. 

As far as having someone go to my vacation getaway to collect values with me (if thats what you meant) not a chance! Ive made the mistake of showing off a mess of fish I caught and telling where I caught them. Know who was at my spot the next day? And that not bad enough- he told of my spot. By the third day- it was no longer my spot.

I don't think my judgement is clouded at all- I do get information (newly learned) filed away in the wrong drawer sometimes, though. Im certain that I have managed to kill my other brain cell somewhere along the past rough and rowdy days of my youth. Does me no good, but I regret not paying any attention to my 10th grade chemistry teacher- I was surrounded by 10th grade girls! 

I still maintain my good looks by being safe and do not attest to being smart(not among this crowd of brainiacs) too. :} You guys are great! Thanks.

Core


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## butcher (Nov 8, 2013)

I am having a hard time focusing with so much written in one post, trying to weed out whats going on here.
( :lol: those poor guys who try to read my long rambling posts).

What i did see in the post is you reduced something with copper out of solution (with ore besides gold a few other things can be reduced with copper metal), but what confuses me more is then you mention then using zinc to cement more,(which would cement a slew of metals or compounds from the solution, was it this material from the cementing zinc you melted?

oxides would not be a problem for an assay.

Ore can get complicated.
Knowing what it is composed of can help to understand how it will react chemically.

sometimes roasting with a little salt can help later when leaching ore,depending on the composition of the ore, but then again at roasting temperatures around 800 deg the chloride can form chlorine gas and dissolve your gold which then goes up in smoke as yellow fumes (which can condense out as yellow liquid or turn what it condenses on violet with gold, if you suspect chloride in the ore roasting may prove a way to lose the gold in the ore.
Chloride in gold ore are normally more rare but if form old ocean not unheard of,
if chlorides were involved in the it can make the gold volatile,

Action mining Has a flux for chloride ore, I am not sure what it is composed of (could be just a high sodium carbonate flux, silver powder, charcoal, lead oxide,and borax ?), I am not skilled enough in assaying, but someone who was could figure it out or determine a flux recipe to use. 
Action Mining sells a flux for chloride ore 
http://www.actionmining.com/fluxgoldchloride.pdf

But here again without knowing the composition of your ore your just spinning your wheels, a good professional assayer should be able to determine the gold content, and analysis of the ore can help to determine what you are working with.

If a good assayer cannot get gold out of the ore it is doubtful you will get any out of the ore.

If I suspected the ore was a chloride ore, I might try to put some into solution with H2SO4, dilute then add some silver nitrate to the solution, if it had chloride I would see a white cloud or white precipitant of silver chloride if the ore in fact did contain chlorides.


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## freechemist (Nov 9, 2013)

Butcher suggests:

_"If I suspected the ore was a chloride ore, I might try to put some into solution with H2SO4, dilute then add some silver nitrate to the solution, if it had chloride I would see a white cloud or white precipitant of silver chloride if the ore in fact did contain chlorides."_

Silver sulfate (Ag2SO4), at room temperature, is only sparingly soluble in water. Thus, adding silver nitrate solution to diluted aqueous sulfuric acid, may well lead to crystallization of colourless silver sulfate.


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## butcher (Nov 9, 2013)

Good point Freechemist,

Although I believe the test would still work, if chloride were involved, the H2SO4 should put chlorides in solutions making HCl, and silver in the silver nitrate solution should form a white cloud, even if some of the silver formed a sulfate.

but with this in mind, the sulfate ions although I do not believe would cause much problem lets try another test just in case I am wrong (wouldn't be the first time).

Chloride test for ore
grind fine a pea size sample of ore, place in test tube, with 2ml H2O (known to be chloride free), add about 8 drops 70% HNO3 bring to low boil and cool.
(Note make observation of the reaction when nitric is added, if carbonates were involved the solution will effervesce bubbling carbonic acid and CO2, if this is seen carbonates are involved which will also precipitate a white silver carbonate in the test with silver nitrate).
when solution cool add several drops of silver nitrate solution, a white cloud will form of silver chloride if chloride were involved (if free of carbonate see note above).


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## core (Nov 11, 2013)

That is a nice set of tools. It ought to keep me busy for awhile, and answer mostly all of my questions. Thanks guys.

sincerely,
core


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