# Flux mystery



## amesametrita (Jan 15, 2013)

Hi, dear forum members!
I refine karat gold using inquartation with silver and parting in nitric for a long time.
The result is consistent *996+* which is enough for my goals.
Contaminant is only silver.
Sometimes bleaching with KNO3
Melting is in a gas kiln.
I tryed fluxing using the forum recepies to achieve *999*

The first one is by *4metals*.
2 pounds Anhydrous borax glass (no waters)
1 pound Soda Ash
1 pound Diatomaceous earth (silica)
1 pound Manganese Dioxide
1/4 pound Flurospar (calcium fluoride)
1/4 pound Calcium oxide (CaO, Lime, Type S, Unslaked)
No results.
Fire assay - no improvement. XFR - no improvement.

The second one is by *Rick. "The Rock Man"*.
3 parts Sodium Carbonate. (Soda Ash)
1/2 part Borax. 
1 part Silica.
1 part Manganese Dioxide.
1/4 part Fluorspar. (CaF2, Calcium Fluoride)
1/4 part Calcium Oxide. (CaO, Lime, Type S, Unslaked)
No results.
Fire assay - no improvement. XFR - no improvement.

Premixing, no moisture.
Slow heating, fast heating, prolonged boiling...
Nothing works.

Any advices?

Best regards!


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## etack (Jan 15, 2013)

You could try AR and no flux to see better results. what is the end use of your gold? 

Eric


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## amesametrita (Jan 15, 2013)

It is a king of scientific experiment.
To understand how stupid I am 
So I want to achieve exactly fluxing result.

No idea about end use of the gold.
Just selling it to a dealer.

AR purification is not economically feasible in the place I live.


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## etack (Jan 15, 2013)

If you get .996 the you are alright to sell to a dealer. Just make sure they can test that high.

experiment away goldsilverpro might be able to help with cleaning gold with flux. that's an OLD argument on this board. Sorry don't want to stir the pudding. :lol: 

Eric


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## MysticColby (Jan 15, 2013)

I wouldn't expect any flux to be able to remove silver impurities from gold. copper, maybe. but not silver.
flux collects solid parts from melts (such as metal oxides, which generally have a higher melting point than the pure metal).
silver oxide converts to elemental silver when heated, so it does not form an oxide.
I say maybe copper because that does form oxides.

you need to refine if you want higher purity. melting does not generally refine.


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## Westerngs (Jan 15, 2013)

As MysticColby indicated, you will have a hard time achieving 0.999 purity fluxing to remove silver.

About the only thing I can think of that you might try is adding salt to your flux to see if you can slag off the silver as a chloride. I guess you could call it a variation on the Miller process. Again, I think you will have a hard time getting 0.999 gold


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## butcher (Jan 15, 2013)

I agree with Mystic, silver is not a metal that would oxidize easily due to its position it the reactivity of metals, and any flux that would oxidize silver I believe would also oxidize the gold and cause loss such as chloride in the flux.

I do not quite understand, you can in-quarter, and part with Nitric, but you say you cannot finish and refine with aqua regia, or another solvent for the gold, or that is not economically feasible, Here for me the nitric is more expensive, so the part of the process you are doing is what cost me the most.


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## Harold_V (Jan 16, 2013)

I'm of the opinion that it will be difficult to improve the quality if the contamination is silver. It has long been recognized that traces of silver behave much like gold, and is difficult to separate from gold, even when dissolving the gold. 

I am not a chemist, nor do I profess to understand well the function of soda ash, but I am a firm believer that including soda ash in a flux that is intended to purify is a mistake if the end product is to be pure gold. That would be particularly true in view of the fact that soda ash is advised for reducing silver chloride in the furnace. To add to that, my years of experience in cleaning melting dishes with soda ash, to me, is evidence enough that any traces of metal that may be present in the material will simply be melted and still report in the material, as your experience has shown. 

If you care to experiment with flux as a method to improve gold quality, two things are important. One of them is an oxidizing agent, so traces of base metals are reduced to an oxide. The other is borax, which absorbs the oxides. Fluorspar can be used to thin the flux, but most likely would not be a requirement for this particular application. 

I would suggest that you try melting with JUST borax, and an oxidizing agent (salt peter has been suggested in the past). If you find the flux discolors upon melting, pretty good sign you're picking up some contaminants, and your quality may be improved. 

Personally, I found the key to high quality gold, assuming you're chemical refining, was to dissolve the gold, filter, precipitate, wash well, then repeat the process. A second refining has the potential to yield very high grade (better than 9995) gold. My routine was to double refine all of my gold, which I did as a matter of pride. I wanted to be recognized as a competent refiner. 

Harold


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## nickvc (Jan 16, 2013)

I'm take a slightly different attitude to many on the forum and I'm a great believer in only doing the minimum work needed to reach the goal I require. I guess that your gold dealer doesn't care what your gold assays at so long as you get 995 or better and won't pay anymore for 9999 so there's no point to refine further in my opinion, if this is your business then definitely not, but maybe the way the Asian jewellers refine their metals might work, they use copper to inquart which is much easier to remove and if it does still report in your gold then the fluxes might do the job. The downside is it requires much more nitric and any silver in the material will need to be cemented out, the copper could be recovered and reused by cementation with steel but I'm not sure the extra work and acid costs would be worth the effort. K.A.Driver did an experiment using only nitric and achieved excellent purity but again it's takes more time and probably more acids which for you might again be a waste of effort and acid costs if you can't achieve a higher price.


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## amesametrita (Jan 16, 2013)

nickvc said:


> ... and I'm a great believer in only doing the minimum work needed to reach the goal I require. I guess that your gold dealer doesn't care what your gold assays at so long as you get 995 or better and won't pay anymore for 9999 so there's no point to refine further in my opinion...



Exactly. It is economically unfeasible to refine from 996 up.



Harold_V said:


> I'm of the opinion that it will be difficult to improve the quality if the contamination is silver. It has long been recognized that traces of silver behave much like gold, and is difficult to separate from gold, even when dissolving the gold.



This was my point of view as well.
Until I found a lot of mentions of 4metals' recipe here.
The point is to use *Manganese(IV) oxide*.
As super strong oxidizer.

After I found Rick's composition, again with *MnO2*

And tried...
And *failed*...


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## HAuCl4 (Jan 16, 2013)

amesa: 

Did you melt your inquarted/leached with nitric, 996 gold, and THEN used the 4metals flux?.

The flux is supposed to be mixed well and then combined well with the powdery gold, then heated slowly (otherwise it will spill over the crucible). Melting only at the end of all reactions. I pour out the (reacted) flux liquid before the gold melts (about 700 Centigrade), then put the crucible back in the furnace to melt the gold.

When I have used the flux, it has worked well (i.e. 9995+ result).

I used 77/23 inquartation instead of 75/25 many times, and my metal of choice has been copper or zinc or a combination of both. I doubt any of what is said in this last paragraph has any relevance on the results.


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## amesametrita (Jan 16, 2013)

HAuCl4 said:


> Did you melt your inquarted/leached with nitric, 996 gold, and THEN used the 4metals flux?.



Correct.



HAuCl4 said:


> The flux is supposed to be mixed well and then combined well with the powdery gold, then heated slowly (otherwise it will spill over the crucible). Melting only at the end of all reactions. I pour out the (reacted) flux liquid before the gold melts (about 700 Centigrade), then put the crucible back in the furnace to melt the gold.



I thought that contaminant survived nitric is entrapped behind gold shield and should be melted out before flux can play.
Ok, will try without melting.



HAuCl4 said:


> and my metal of choice has been copper or zinc or a combination of both.



Looks like this is the main difference.
It's much easier to slug out copper and zinc.
And you don't need Manganese Dioxide for this task.

I must use silver for inquartation to remove PGM.


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## HAuCl4 (Jan 16, 2013)

amesametrita said:


> I must use silver for inquartation to remove PGM.


That's what 4metals used, actually sterling silver. I believe silver is what the original guys that discovered the method by mistake used too.

"The trick" is to mix well the flux with the gold powder after inquart. I like to get rid of the "dirty flux" before melting too. Silver and also base metals are scavenged into some complex oxides by the MnO2. Of course this happens better at maximum surface area (i.e. before melting the gold).

If you have some tin in your inquarted gold, a 15 minute boil in sulphuric acid, after the nitric acid treatment, will help with the purity.

Also a second, 15 minute boil in concentrated nitric acid under pressure (2-3 bar) will likely bring you to 997, 998 purity. This is unrelated to the fluxing method (also don't melt the gold before the second nitric boil... :lol: ).


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## samuel-a (Jan 16, 2013)

Silver will not form oxide over 450C.
Even if it is trapped in the slag (which i doubt) it could just as easily drain down. Flux is definatly not a bullet proof way to refine gold to higher purity 999+, no matter how you twist it.

Even if you pump Cl to the charge, most likely you would not remove this last bit of silver.
On this subject, i've seen a mention above about NaCl as chlorinating agent, That is not the case. 
Personally, I have melted silver with NaCl many times (from AgCl method) without any loss of silver.


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## HAuCl4 (Jan 16, 2013)

Yet it works...


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## amesametrita (Jan 21, 2013)

4metals original post mentions 30 minute @ 2000F:

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=49&t=6187#p54099


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## kadriver (Jul 25, 2013)

This is an old post, but I have some experience to share. I have had consistent success producing 3 nines (99.9%) pure gold using only inquartation and dilute nitric treatments.

When calculating for inquartation, I use 75/25, but I multiply the calculated amount of silver by 1.1 to increase the amount of sterling I add by 10%. This usually makes some nice pieces that cling together through the whole process.

I then do an initial dilute nitric treatment in a COVERED container for about 1/2 hour with medium heat, drain the liquid into my silver jar and rinse well with distilled water. The liquid I drain off is dark blue.

The second nitric treatment is the same except I turn the heat way up and boil until there are no more brown fumes, and the liquid is at a rolling boil, I remove from the heat, drain and rinse again - this take about 60 to 90 minutes.

The third treatment is the same, but this time I turn the heat up and just let it boil away for several hours - maybe three. By now the acid is only pale blue as most of the silver and base metals were removed in the first two nitric treatments. I pour off the liquid into my silver jar - a heavy Pyrex coffee pot with a glass lid.

The fourth treatment is the same as the third, except I let it boil for up to 6 hours with fresh clear dilute nitric acid. At this point the dilute nitric sometimes turns a pale yellow color, but stannous test turns up negative. I pour the hot clear acid in my silver jar along with the wash water and use it to dissolve more silver later on for my silver cell.

The pieces of inquarted gold are in their original shape and are an orange brown color. I can tell that they are really pure by the color, especially after rinsing and drying.

This process takes lots more time and electricity, but I can count on getting 999 on the assay just about every time.

I've never (yet anyway) had a problem with tin or lead.

I've used this process so regularly that I have lost some proficiency in my refining technique. I used AR to do a refining the other day and left out a step (adding H2SO4) before filtering.

kadriver


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## kannang338 (Aug 18, 2016)

Hi folks,

Currently we are trying to reduce zinc, indium, iron and partly copper in the melting stage with the help of oxidizing flux and oxygen purging.

But we can't able to select the perfect flux and their combinations to oxidize the input material. (4 to 5kg of 22kt gold which is having about 300grams of alloy materials as mentioned above)

Is there any better flux available for effective oxidation to occur.

We recommend the final output have less than 100ppm of the zinc and iron.


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## Lou (Aug 18, 2016)

Heat will cook out the zinc but so too will borax. Silica is a good trap, along with borax, for Fe.

You might consider Miller process.

HAuCl4 is no where to be seen (hope he is well) but he has small batch experience with Miller.


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## houseofsas (Oct 28, 2016)

Does anyone know about the old school assay and the new assay methodology ? I have a complex ore that is supposed to be around 2% gold per tonne got 1 test on it all the other tests show basically nothing, is there a difference in testing for monoatomic and diatomic gold ? Also when taking the raw complex ore, i microwave the ultra fine powder first, what would be a good formula for smelting in a induction furnace to get the best results? Anyone have some going tips at all ?


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## FrugalRefiner (Oct 28, 2016)

houseofsas said:


> Does anyone know about the old school assay and the new assay methodology ?


Can you define these terms for us? What do you mean by an "old school assay", and what is the "new assay methodology" you're asking about?



> I have a complex ore that is supposed to be around 2% gold per tonne got 1 test on it all the other tests show basically nothing,


 :shock: One test tells you you have over 500 ounces of gold per tonne, but all others are negative! :shock: Think about that.

Dave


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## houseofsas (Oct 28, 2016)

Yes I get that , that is why I am asking, I can send the reports for review as its confusing to me. What I believe is there is alteration state in conversion from the mono to di factor which i think the report 1 shows, this is what I would like to ask if anyone knows about this.


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## houseofsas (Oct 28, 2016)

There were not negative there with just minimal ppm results back


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## houseofsas (Oct 28, 2016)

And what I am meaning by old school reports and the new reports is that I have heard that people that understand assay doing before things were done different that how they assay now.


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## houseofsas (Oct 28, 2016)

This is what I am wanting to know.


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## FrugalRefiner (Oct 28, 2016)

I would tend to believe the reports that said minimal ppm.

Dave


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## houseofsas (Oct 28, 2016)

well i kind to tend to not agree as using the microwave i am getting .5% out of it so if there is someone that understands the mono and dio aspect this is where i would like some help


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## Platdigger (Oct 29, 2016)

Curious how you are using the mirco. Stumble on a good flux?


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## g_axelsson (Oct 29, 2016)

If someone is talking about "monoatomic gold" then it is alchemy and that is just humbug.

If you sent a number of samples to assayers and only one comes back with high numbers and talking about monoatomic gold then the only thing they are after is your money. Trying to sell you a special flux that would extract the gold where normal methods would fail, It is a well known scam.

Göran


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## goldsilverpro (Oct 29, 2016)

Anyone using the term monoatomic is either a liar or a person that's been listening to a liar.

There is NO such thing as "new assay methodology." Fire assay has been essentially the same for centuries, with only a few improvements. Anyone using the term, "new assay methodology", and is saying that it is different than traditional assaying is a liar or a person that's been listening to a liar. If a traditional fire assay, done by an experienced assayer, shows only a small amount of gold, that is absolute, 100% proof, that there is only a small amount of gold in the ore. No ifs, ands, or buts. There is absolutely no such thing as "immature" or "embryonic" gold that must be treated differently to make it "mature."

How do you know you got .5% gold in your microwave? Please explain in detail.

We're trying to protect you from scams and the "100% false alchemical chemistry, with no exceptions" that has been around for many centuries.

Please notice the first quote in my signature below, "It is better to hear the rebuke of the wise, than for a man to hear the song of fools." This was posted primarily for people that are getting sucked into alchemical lies - people like you.


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## houseofsas (Oct 29, 2016)

First off Im not promoting fake, you can look up microwave tech, John Milewski or in fact others that are producing, what I am wanting to know is if anyone knows about getting the better results. Im already getting good results and tested by 5 different independent labs, Im not looking for to promote or sell anything , what I am wanting is if someone else is also figuring this out that I can get some proper responses.


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## g_axelsson (Oct 29, 2016)

I did look up John Milewski and he's such a fraud, extracting gold from ground up beer bottles and all.

You won't find anyone here that will help you with your quest, we are recovering and refining real gold and are not dealing with alchemy.

Göran


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