Still shy of 4 nines

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Galaxy419

Galaxy419

Well-known member
Joined
Jan 6, 2015
Messages
70
Location
Royersford Pa
Two different batches of 14 and 10 k scrap both were refined twice and I used Harold's washing technique.
I am still dragging some silver and some copper down. I did use smb on both bathes to precipitate. I haven't used hcl/cl
Enough to feel comfortable with. Don't get me wrong I am not complaining about my results. I just was wondering why I can't get rid of that last bit of ag and cu. I was told my material was fired assayed. Any help or suggestion will be greatly appreciated .
 

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It is what it is Galaxy. That's a pretty good result, and I'd be happy with it. Nice work on the gold.

Remember you're talking about 0.008 g per Kg here between your result and four nines. That's a truly tiny amount of impurity. Edit: or is it 0.08g per Kg? Sorry it's late over here and my maths brain isn't working.

I don't get silver in my assays, only copper. How do you filter out the silver chloride from your solutions and what do you use to wash the silver chloride away from your powder?

I use HCl as per Lou's wash method.

Jon
 
I remember a discussion between the pros I read recently...
from what I remember, two things might help:

1) dillute and filter the solution before precipitation (more silver will precipitate as chloride and can be filtered off)
2) wash with cold concentrated HCl and or cold NH4OH (silver and copper are less soluble in hot HCl or hot NH4OH)

btw. decanting/syphoning from crystal clear solution might be better than filtering through non-high-quality filters.


I hope I got that right.

I have some ideas in regard of the accuracy of the assay, but I don't want to swim out in deep water. But this assay seems not to be as proper as the descriptions of propper assays I read from the pros of the forum.
 
Great purity and nice bars! Need my 8) on to look at that shiny stuff!

That is not a fire assay, it's an XRF assay. Voltage and current is the settings of the x-ray gun.

Göran
 
Thanks everybody for the help and advice I was told it was fire assayed I had 34.1 dwt when I dropped it off to the guy
Who took to the refinery for me and said I lost .1 because it was fire assayed . So was I being lied to? I was told they
Drilled a small hole then melted the material down? I understand he has to make a profit but don't lie or cheat me. I got paid 94% spot and was told spot on 3/10/16 was 1223$ for Troy ounce and I showed him Garfield refinery spot price 1266
For Troy ounce and I am about 99.99% sure that's where he took it. Then he gave me some explanation about second London price then kimox price ? How is a guy supposed to know if he is cheated if he can't even get straight answer on
Spot price ? Maybe time to sell somewhere else. How does one sell gold here on forum? Sorry for rambling on
 
As for washing powder 3x hot distilled h2o then hot hcl til clear ( never tried cold hcl) think I will try that next time. Then a hot wash in ammonia then hot hcl for 5-7 min to make sure I get rid of all ammonia then a final wash in distill h2o
 
Lord god knows i wouldn't dare question You Lou, but i don't see the logic in cold? I know you have talked about a cold solution holds more in the gaseous phase, but the logic from my personal experience doesn't imply that that has an effect when we are talking contaminate removal. Cold hcl doesn't really dissolve copper until an oxidizer is added or the heat is elevated. Think the crock pot method or ap? Copper doesn't dissolve in hcl alone and the solubility of agcl goes up with temperature. In order to get to the contaminate that may be trapped on a molecular level with the gold precipitate crystal that formed you need heat to drive the solution through the material. True some amount of hcl may decompose at elevated levels, but that amount should be musicale compared to the mg of materials that make of the foreign contaminate that needs removed. The contaminate will be removed far before you exhaust the hcl from the rise in temperature of the solution in any considerable amount to be detrimental. Scientifically it might make sense, but practically to me it doesn't.
 
Disagree with me if you like but here my logic (and the science) behind it:

1. AgCl is most soluble in very strong concentration HCl solutions, solutions which are fuming.
2. HCl is a gas dissolved in water. Heating HCl does in fact decrease its [Cl-] content to the constant boiling azeotrope.
3. Ditto with ammonia.
4. Copper contamination in gold is often the same form as silver, as its monochloride from overuse of reductant. Do an experiment and make cuprous chloride and then try dissolving it in concentrated HCl and heating. Watch it dissolve and reappear. Same with AgCl. Measure the specific gravity of the acid and you'll see why.

Heat makes both muriatic and especially ammonia less effective.
 
I must admit I was sceptical until I saw gold powder washed in cold HCl, it works, better with a magnetic stirrer, but yes it works.
As to your assay, so called, result I seriously doubt an xrf can tell if it's 9999 or not, and the industry standard or standards are 995 or 999 for gold so you are above the required assay for good delivery 8)
 
nickvc said:
I must admit I was sceptical until I saw gold powder washed in cold HCl, it works, better with a magnetic stirrer, but yes it works.
Click to expand...

If I recall correctly, skeptical was an understatement. the look of utter disbelief was profound... 8)


Jon
 
I just researched the internet for the lower detection limit for tetraammine copper and found that 1mg in one case and in another case 1,2708 mg per ml solution were detectable by photometry. If my math is correct, this would mean, it can detect 00,01% copper in a 10g 99,99% gold sample.

right now, I can't see any really practical use, since we can't use this on gold solutions, only on the filtrates when washing elemental gold powder, just thought it to be interesting in this context
 
solar_plasma said:
I remember a discussion between the pros I read recently...
from what I remember, two things might help:

1) dillute and filter the solution before precipitation (more silver will precipitate as chloride and can be filtered off)
2) wash with cold concentrated HCl and or cold NH4OH (silver and copper are less soluble in hot HCl or hot NH4OH)

btw. decanting/syphoning from crystal clear solution might be better than filtering through non-high-quality filters.
Click to expand...

Couple of things Bjorn if I may?

Firstly when doing a recovery drop from a batch of let's suggest ceramic processors for example, I don't dilute the AR and I keep water away from it as much as possible. The logic being my waste is lower because when I actually refine the gold in the next step I use much much less liquid therefore diluting that produces far less overall waste.

If you have 12 litres of AR in the recovery stage, then diluting that by a factor of even 50% adds another 6l to your waste. Diluting 250ml by the same factor only adds another 125ml.

I think you raise a great point about decanting the crystal clear liquid, and I do this too in the recovery stage even though I do use high grade vacuum filtration with excellent filters. I leave the residue in the bottom of each flask of AR and combine those and filter those together, thereby reducing the requirement for filtration. When performing the true refine, I do filter the complete solution but by this point it is almost crystal clear prior to filtration.

Jon
 
I agree completely, Jon.

I focused more on the quite pure gold of the OP, if he wants to rerefine.

Regarding e-scrap, I do not really count the recovery stage and I do not spend extra effort making a great art of it. So, with Chris' definition of "refining", I am triple refining this kind of material - I would never dillute a dirty solution, there will be drag down anyways.
 
Very true Bjorn.

If asked that question - with a purity that he has already I wouldn't re-refine it. The inherent "loss" in the process of doing to gain that extra 9 wouldn't be worth it and aside from the ability to say he's done 4 nines there would be no financial gain.
 
It is capable of that precision (4N) if it has high excitation energy (think 3-4 kW), is on a prepared sample (think a cast puck with a milled flat, etched surface). So basically I mean bench top wavelength dispersive x-ray fluorescence. It's most useful on homogenous powders (like brazing atomizate about to be made into paste).

Here's an example of an instrument that can do:

https://www.thermofisher.com/us/en/home/industrial/spectroscopy-elemental-isotope-analysis/oes-xrd-xrf-analysis/x-ray-fluorescence-xrf/arl-performx-wdxrf-available-ucco-30-x-ray-tube.html
 
Lou said:
It is capable of that precision (4N) if it has high excitation energy (think 3-4 kW), is on a prepared sample (think a cast puck with a milled flat, etched surface). So basically I mean bench top wavelength dispersive x-ray fluorescence. It's most useful on homogenous powders (like brazing atomizate about to be made into paste).

Here's an example of an instrument that can do:

https://www.thermofisher.com/us/en/home/industrial/spectroscopy-elemental-isotope-analysis/oes-xrd-xrf-analysis/x-ray-fluorescence-xrf/arl-performx-wdxrf-available-ucco-30-x-ray-tube.html
Click to expand...
It's not only the x-ray tube that affect the precision, it's the technology of the detector. Most (if not all) simple elements uses an EDS (Energy Dispersive Spectromemetry) detector, where a silicon crystal have electrons knocked off to measure the energy of an x-ray from the target, giving a ruler with an 8.1 eV step.
While WDXRF uses salt crystals as a diffraction grating, reflecting a narrow energy band into a detector, giving a very narrow energy gap that is sampled. By turning the salt crystal the whole energy spectra can be scanned. That also demands higher intensity of the x-ray gun as most of the fluorescent x-rays are filtered off in the WDXRF while EDS measure every x-ray that strikes the detector.

If the material is not flat and homogeneous the result will be off since geometry affects how well x-rays can leave the material and variations in composition affect absorption in different wavelengths of the x-rays leaving the material, throwing off the statistical calculations.

A bit technical... sorry about that. 8)

Göran
 
I am currently panning out micron gold from my soils and sands. mountain sides of clay and silt , as well as hard rock quartz with gold traveling veins, I have hills with heavy iron stained quartz and granite, colored blue, gold, red ,yellow, green or just very clean white.they are stuck in the base of the mountain in the walls or sprouted out the mountain top, looks like theyre is also a lot of limonite. id say quite a decent amount of gold in almost all the rocks.there is this type of golden sand minimal iron in it. in large firm yet brittle sand structured mountain areas.it seems like its majority gold yet cant seem to wrap my mind around that concept.i throw some of the yellow gold sand in with say some gold from quartz vein and the sand is the heaviness of what I know is gold. when it rains and the little trail of water runs down the property, a very gold colored deposit forms in the deeper puddle imprints of the floor if any trail at all that is.is such a thing possible? with a torch ive burned out metals straight outve rocks, these vibrant blue beads started to form ,firwst as little beads and grew larger until I got them to spill off and eventually cooled ibeautiful silvery and some reddish golden metals .anyways I have a 20lb propane and a bbq, im looking to fire assay some of what I panned out, mostly micron gold from the soils and sand formations due to the easiness of pulverizing that type of material.can I get the temperature needed in an enclosed bbq. I plan on mixing my assay materials with borax,lead ,aand perhaps some flour?`what is a good source of lead I can get my hands on?..i iknow there is plenty in the rocks but the silver metals are hard for me to differentiate. obviously a professional refinery is the way especially to get it done correct and get me some good start up money..im looking into mailing in a ten lb batch assay to a man in Nevada , hell fire assay ten pounds of material plus an atomic absortion assay for $175.`i was gonna send out ten pounds of what I panned out from the soils and hardrock. Id like opinions on everything ive mentioned as well as questions if more are needed to better explain what im working with ....thank you
 
cherrypicktheplacer said:
I am currently panning out micron gold from my soils and sands. mountain sides of clay and silt , as well as hard rock quartz with gold traveling veins, I have hills with heavy iron stained quartz and granite, colored blue, gold, red ,yellow, green or just very clean white.they are stuck in the base of the mountain in the walls or sprouted out the mountain top, looks like theyre is also a lot of limonite. id say quite a decent amount of gold in almost all the rocks.there is this type of golden sand minimal iron in it. in large firm yet brittle sand structured mountain areas.it seems like its majority gold yet cant seem to wrap my mind around that concept.i throw some of the yellow gold sand in with say some gold from quartz vein and the sand is the heaviness of what I know is gold. when it rains and the little trail of water runs down the property, a very gold colored deposit forms in the deeper puddle imprints of the floor if any trail at all that is.is such a thing possible? with a torch ive burned out metals straight outve rocks, these vibrant blue beads started to form ,firwst as little beads and grew larger until I got them to spill off and eventually cooled ibeautiful silvery and some reddish golden metals .anyways I have a 20lb propane and a bbq, im looking to fire assay some of what I panned out, mostly micron gold from the soils and sand formations due to the easiness of pulverizing that type of material.can I get the temperature needed in an enclosed bbq. I plan on mixing my assay materials with borax,lead ,aand perhaps some flour?`what is a good source of lead I can get my hands on?..i iknow there is plenty in the rocks but the silver metals are hard for me to differentiate. obviously a professional refinery is the way especially to get it done correct and get me some good start up money..im looking into mailing in a ten lb batch assay to a man in Nevada , hell fire assay ten pounds of material plus an atomic absortion assay for $175.`i was gonna send out ten pounds of what I panned out from the soils and hardrock. Id like opinions on everything ive mentioned as well as questions if more are needed to better explain what im working with ....thank you
Click to expand...
It's VERY difficult to read such a large paragraph. You're more likely to get a response if you'll break it up in several, so readers can establish a reference point.

Just sayin'

Harold
 

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