# Murphies Law



## dragoneproducts (Dec 19, 2016)

It's been a while since my last post here. At, the time I had become a member, I was in search of platinum group metals; in CA. I had researched this, as a child. Last year, I finally remembered the area I wanted to (assay) prospect. The area is in a national forest, part of a wilderness act. I had read parts of a mineral journal from the late 1800's that led me to believe, that where there are diamonds, gold, and other useful metals, that there would also be, as described in this journal, platinum group metals. I arrived in CA ready to dredge in 2009. The use of a dredge was outlawed, three months later. I have and had done, hundreds of hours of research for processing noble metals and thier constituants nano particles. I am flustered, exasperated, and generally dissapointed in my effort(s). I am better than what my mis-steps have caused. My process started as an acid assay. I was not looking for purity, just parts per million. I have/had 3 1/2 pounds of (alleged) nickel ore from a well known river of 'gold.' I soaked my material in muriatic acid for a week. Poured off the acid and rinsed a few times. I did not let the material dry completely. I then prepared to dissolve the base metals further with -70% nitric acid. During the process, it seemed as if the nitric acid was reacting as planned. I gathered the remaining, floating silt, that I thought, had not reacted to the nitric acid, rinced, settled and dried for XRF assaying. I received my results in a few days. Opening the letter, I was shocked, not upset, just shocked. An abundance of iron, tin and so on. A fair among of silver and small amounts of, both rhodium and zirconium ppm. 0 ppm for gold, platinum, palladium, iridium/osmium and ruthenium. Rhodium without any other pmg's, odd; no gold either, from a well-known gold bearing area in the mother load of CA. I almost new immediately, what had happened. My clue was the rhodium content, with the absence of the other noble players. Alas; I had made a week aqua-regia. (right?) Because I already know that gold is there, I am only concerned at this time, about the missing platinum. It is now almost freezing at night. I find the ammonium chloride I will need to 'drop' the platinum. My containers include, hydrochloric acid; 2 1/2 liters of nitric acid; and distilled water. Totalling around 4 gallons. Upon adding my powdered ammonium chloride, nothing happens. I wait for 24 hours. I have some, a very minute amount; of a pinkish-brown silt. I assume it is a platinum group element. After this fail, I research some more. Apparently, My liquid is too dilute. I am not working in a professional environment, I am using caution and safety. For my end result, I only need to know, if the ptatinum exists, before Murphy gets me again. "Murphy" wants me to get 'urea'; skip the (alleged) platinum, and get the gold. Any advice or comments, would be, greatly welcomed....


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## FrugalRefiner (Dec 19, 2016)

dragoneproducts said:


> Any advice or comments, would be, greatly welcomed....


Get an assay so you know what you're working with before you kill yourself.

I'm not trying to be a jerk. My advice is quite serious. If you're throwing several pounds of unknown ore into several gallons of acid, it would be very easy for you to kill yourself or someone downwind/downstream of you.

Dave


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## jeneje (Dec 19, 2016)

dragoneproducts said:


> I had made a week aqua-regia. (right?) Because I already know that gold is there, I am only concerned at this time, about the missing platinum. It is now almost freezing at night. I find the ammonium chloride I will need to 'drop' the platinum. My containers include, hydrochloric acid; 2 1/2 liters of nitric acid; and distilled water. Totalling around 4 gallons. Upon adding my powdered ammonium chloride, nothing happens. I wait for 24 hours. I have some, a very minute amount; of a pinkish-brown silt. I assume it is a platinum group element. After this fail, I research some more. Apparently, My liquid is too dilute. I am not working in a professional environment, I am using caution and safety. For my end result, I only need to know, if the ptatinum exists, before Murphy gets me again. "Murphy" wants me to get 'urea'; skip the (alleged) platinum, and get the gold. Any advice or comments, would be, greatly welcomed....


First, did you test the solution for PGM's or Gold with Stannous? Second, How do you know that there are Platinum group metals in the ore without an assay? Third, weak AR is not going to do anything in this situation, the leach is going to be eaten up by other metals, such as Iron for one. So, if, any gold did dissolve it has cemented back out of solution. 

Finally, if I were you, I would stop before I got hurt, or hurt someone else. You really need to do a bit more research on the process you have chosen.

Good luck,

Ken
edited to add one other note: PGM's are extremely dangerous, so if they are present make sure to have your PPE on.


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## dragoneproducts (Dec 20, 2016)

Dave; I certainly did not intend to cause any alarm. 

Obviously, I need to clarify a few things. The nickel ore, is in the form of black sand concentrates, from a 3 month prospecting trip. The concentrates are non-magnetic. 

My next step will by the stannos test, as recommended by jeneje. I will take things slow and keep you posted. If my aqua-regia is to dilute, will I get a proper reading?

Thanx for replying, and ensuring that my process is being done safely.


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## nickvc (Dec 20, 2016)

As Ken has pointed out even if you did dissolve any precious metals the presence of base metals in your assay would mean any PMs would have cemented back out and should have shown up on your results, the fact you didn't find any suggests strongly that there were none present to start.
Instead of wasting time, chemicals and risking your health I would suggest having an assay done as Dave has suggested, just because an area has PMs does not mean the whole area wil, yield them they could well be in concentrated deposits which your sample didn't come from.
It seems that miners have very dogged views and do not believe the proven results however many times they are shown but stick to their view that they have found what they were looking for.


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## butcher (Dec 21, 2016)

The key to recovery of these metal is density.


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## upcyclist (Dec 23, 2016)

If your assay comes back with some recoverable PM content, and does NOT contain anything that reacts poorly with acid (in terms of your health), then check your technique as well. I don't see where you created aqua regia other than a reference to soaking in HCl, not drying completely, then adding nitric. Normally, an HCl soak would remove some base metals, then you would roast your material to remove chlorides before moving on to nitric. Then, once you've removed your base metals, silver, and palladium with the nitric, you can move on to AR.


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## butcher (Dec 23, 2016)

To mine these metals your best bet is mining the bedrock of creeks and rivers or ocean black sand deposits, the gold or other precious metals will be collected and separated from the tons of gangue material by means of gravity separation by their density.

Unless you have a lot of skill in mining finding these in ore (rock) and recovering them is not likely.


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## dragoneproducts (Dec 23, 2016)

upcyclist said:


> If your assay comes back with some recoverable PM content, and does NOT contain anything that reacts poorly with acid (in terms of your health), then check your technique as well. I don't see where you created aqua regia other than a reference to soaking in HCl, not drying completely, then adding nitric. Normally, an HCl soak would remove some base metals, then you would roast your material to remove chlorides before moving on to nitric. Then, once you've removed your base metals, silver, and palladium with the nitric, you can move on to AR.


My intension, was to complete a simple assay and an unpure value. To the best of my knowledge and in a reasonable budget, I roasted my concentrates (nickel ore?) from a well documented area for gold, and as posted by mindat, platinum group elements. I soaked to remove the lower base metals, knowing that silver and palladium would be dissolved, (I plan to extract this later) I then added nitric to dissolve the rest of the concentrates knowing I would loose some values and attain unwanted ganges in my sample. The queer part to my process, is both, in the gold and rhodium content in my paided for, analysis. " 0 ppm=gold and platinum; 1,308 ppm=silver; 125 ppm=rhodium." I understand the proper procedures and the desired outcomes for elemental science. I wanted to try this approach; one, for a quick value assay, and two, for a faster, unpure process. With the remaining values and gange to be delt with at a later time. Going after the PGE's, and not the gold, and not seeing the gold turn-up, is extremely perplexing. 0 parts per million, in a known 'motherload' area in Plumas CA. This is why my assumption leads me to believe I still have values somewhere, another assay would be great, but I need to understand, first hand, what it takes to fix or find my values. Therefore; I push forward and gain first hand knowledge.

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## jeneje (Dec 24, 2016)

dragoneproducts said:


> upcyclist said:
> 
> 
> > If your assay comes back with some recoverable PM content, and does NOT contain anything that reacts poorly with acid (in terms of your health), then check your technique as well. I don't see where you created aqua regia other than a reference to soaking in HCl, not drying completely, then adding nitric. Normally, an HCl soak would remove some base metals, then you would roast your material to remove chlorides before moving on to nitric. Then, once you've removed your base metals, silver, and palladium with the nitric, you can move on to AR.
> ...


Okay, I am going to make this simple for you. Take say 500 grams of the concentrates, separate it with wire mesh sieves starting at 20 mesh going to 100 mesh, (20, 40, 60 ,100) Put them into separate container and sent them to an assay company, (_Lou, 4metals and few others members here may be able to do the proper assay for you_) This will cost you a little money. 

Now, they can fire all four samples, this will give you a better view of what you have and how to go about getting it out. Sulfides out west are very prevalent in ore. Arsenic, tellurides along with other metals have to be removed first before going after the money. 

From what you are saying you have Silver mixed with Rhodium, Rhodium for the hobbyist refiner is going to be a challenge to recover and more of one to refine without the proper knowledge and equipment. Mixing up a AR solution and just let it set with Platinum group metals other than Palladium is not going to dissolve to any great extent. These type metals need heat and a lot of it to break down. I understand your frustration here but, learning something new always has a curve to it. Safety should always be FIRST and FOREMOST!

One other thing to note is Silver DOES NOT dissolve in AR.

Ken


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## jeneje (Dec 24, 2016)

> This is why my assumption leads me to believe I still have values somewhere, another assay would be great, but I need to understand, first hand, what it takes to fix or find my values.


I just re-read your post. Why are you assuming you still have values? If you still have your solutions, place a piece of copper in it and ANY VALUES will cement out as black powders. That is why you need to have someone do a proper assay on the material. Just because it was a mother load area does not mean there is still anything of value there.

Ken


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## dragoneproducts (Dec 24, 2016)

butcher said:


> To mine these metals your best bet is mining the bedrock of creeks and rivers or ocean black sand deposits, the gold or other precious metals will be collected and separated from the tons of gangue material by means of gravity separation by their density.
> 
> Unless you have a lot of skill in mining finding these in ore (rock) and recovering them is not likely.


Hey butcher; Adside from all of the great advise and encouragement from yourself and many others on this forum, I want to express the reasons I have progressed in my assaying, in the manner I have. The original forty-niners new nothing of platinum group metals. Therefore; my intrigue of the motherload area of CA. Although; I have yet, too find the sperrylite vein, I believe, truly, that I will. You might think, if there was one or that there is sperrylite, that the major mines would already have claimed it. I am prospecting the wilderness act of a national forest. No chance to grease pockets on the area, since the rivers flow to a source of drinking water. I have been trying to do things my way, for two reasons. I want to experience the joy of knowing, that my own craft and knowledge, fostered my discovery of values. The other reason is to be prepared to change my mode of operation to suit the situation. If I truly come across a sperrylite vein and the area can't be claimed, and no machines can be used, including metal detectors; than I will need all of the possible trouble shooting abilities I can find. I just wanted to let you, and the other great 'minds' on this forum know, I have heard you all load and clear. I thank you all for your guidance and reassurance. If my values show up, I will post them, and get busy on the studying of the procedures I will need. Once again; thank you and Happy Holidays, too all !!!!!!!!

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## butcher (Dec 24, 2016)

Many of the Miners of old did know about, and recovered the PGMs when gold mining, some of the mining practices of the day were not really suitable to collect the small amount of platinum and gold was what they were after.


dragoneproducts, sperrylite is an arsenic-based ore, arsenic and aqua regia releases a deadly gas, in which you can easily poison yourself...

There are PGM's in our area your best bet of finding any is through panning the creeks and rivers where these metals are concentrated naturally by their density, and can be recovered by the fact they are heavier than any of the other gangue minerals.

I doubt you will find any pockets of ore that would hold enough value to mine (hard rock).

A professional fire assay will be your best bet.



Simple field tests of the ore can be made (preliminary to an assay), using fusions and or wet chemistry, or other methods can be used to detect values in the ore... These will not tell you if the ore is rich enough to spend money and labor on mining but can be an indication some valuable metals are there.

Roasting of the crushed sample, to remove volatiles (sulfides, arsenic...), the ore can treated with different methods, such as it could be roasted with salt NaCl to help form chlorides of many of the metals involved (some of which the salts of some metals also become volatile in the process, A leach in aqua regia and testing with stannous chloride...

Roasting the ore unlocks the bonds of sulfides, arsenic or other bonds, but it also releases very deadly compounds, take precautions for your health or life, gain an understanding of the dangers you are dealing with so you can protect yourself.

https://www.pdf-archive.com/2015/02/17/you-can-smelt-too/you-can-smelt-too.pdf


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## dragoneproducts (Dec 24, 2016)

butcher said:


> Many of the Miners of old did know about, and recovered the PGMs when gold mining, some of the mining practices of the day were not really suitable to collect the small amount of platinum and gold was what they were after.
> 
> 
> dragoneproducts, sperrylite is an arsenic-based ore, arsenic and aqua regia releases a deadly gas, in which you can easily poison yourself...
> ...


You mentioned "in our area" in your post. Where are you from?

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## butcher (Dec 24, 2016)

Southern Oregon / Northern California


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## dragoneproducts (Dec 25, 2016)

butcher said:


> Southern Oregon / Northern California


Well, that's not exactly, 'an ore's throw,' from where I am, Chico CA. but relevant. I think, I may have jumped on a soapbox, in my posts. I researched slot about the PGE's years ago, and yes I remembered the arsenic and sulfides when I began to process my concentrates. I do roast first, outside. I wprk my acids and salts correctly as well. I understand thay only a true, studief, chemist shiuld be handling these things, but I am really as safe in my practice, as if OSHA was looking over my shoulder. The concentrates are coming out of a branch of the Feather River. Plenty of gold, by hand and sluice. The speculation I had arrived at, in terms, of the knowledge the miners had, or the lack thereof, led me to the area I am in. I am not saying they were dumb or ignorant, just not as informed or interested in PGE. Imagining them, back then with plenty of gold at thier fingertips and a very difficult, yet rare and noble material, that was complicated to work with, gold would be the prefered mined metal. MINDAT; (mineral database) links a reference to known PGE's in a mining journal from sometime, around the 1880's. The knowledge was there, but when you could pick up an ounce a day, in gold, with your hands, I think it (platinum) became irrelevant. I am 100% sure that a sperrylite vein exists in the area (10 mile radius) There is also plenty of PGE's in Trinity River, according too MINDAT. 

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## butcher (Dec 25, 2016)

The platinum metals is so much rarer than gold, it was collected with gold during panning, gold was the target metal they mined, the platinum group was so rare it was never the target metal of mining, I cannot remember where I seen the reports, but I have seen old mining report or records of the amount of metals mined in my area here in oregon and seeing the mined ounces of platinum mined listed (along with gold for that time period time), the platinum was not the target metal but was only a byproduct of gold mining. there was not enough of this metal to target it in a mining operation.

https://pubs.usgs.gov/circ/1934/0008/report.pdf
https://pubs.usgs.gov/mf/1994/2270/report.pdistrict.com/mining/platinum-josephine-county-oregon.htmdf
http://www.jeffersonminingdistrict.com/mining/platinum-josephine-county-oregon.html

http://www.oregongeology.org/pubs/og/OBv35n09.pdf
http://raregoldnuggets.com/blog/?p=1705
http://www.goldrushnuggets.com/orbepl.html


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## dragoneproducts (Dec 26, 2016)

butcher said:


> The platinum metals is so much rarer than gold, it was collected with gold during panning, gold was the target metal they mined, the platinum group was so rare it was never the target metal of mining, I cannot remember where I seen the reports, but I have seen old mining report or records of the amount of metals mined in my area here in oregon and seeing the mined ounces of platinum mined listed (along with gold for that time period time), the platinum was not the target metal but was only a byproduct of gold mining. there was not enough of this metal to target it in a mining operation.
> 
> https://pubs.usgs.gov/circ/1934/0008/report.pdf
> https://pubs.usgs.gov/mf/1994/2270/report.pdistrict.com/mining/platinum-josephine-county-oregon.htmdf
> ...


Respectfully; the prospectors/miners gathered their gold; blacksands, kept their gold and bulk sold, the blacksands too, guess; the refiners, who made huge profits to process the PGM's. Yes they gathered it. 

Notice that at the peak of the 49ers, the first world war started. Who wouldn't give their iron and nickel for the benefit of pride in your country? They also didn't have access to the many reagents and the processes to pull off a profit, therefore opening the path to simply give it to refiners for a penence of the value. Ya; they really can be that diabolical. They have done far worse for war....Did you see the spike in rhodium in 2009? From $2000.00 - $10,500.00 in a matter of a month, only to drop back down too $2000.00

If that ever happens again, I for one, will be ready....

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## jeneje (Dec 26, 2016)

dragoneproducts said:


> Did you see the spike in rhodium in 2009? From $2000.00 - $10,500.00 in a matter of a month, only to drop back down too $2000.00
> 
> If that ever happens again, I for one, will be ready....
> 
> Sent from my X301 - Locked to Life Wireless using Tapatalk


 :shock: How do you plan on getting this material to the refiner or, are you going to refine it at your facility? 

Ken


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## dragoneproducts (Dec 26, 2016)

jeneje said:


> dragoneproducts said:
> 
> 
> > Did you see the spike in rhodium in 2009? From $2000.00 - $10,500.00 in a matter of a month, only to drop back down too $2000.00
> ...


Hmmm facility; I will, at sometime, have a facility, but as if now, I don't. It may be a fee years before it goes back up, or the next rush for it. I figure, since, I get gold and platinum, I will set the rhodium aside, in a pure form, and cash the rest. Saving the iridium/osmium just in case......

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## butcher (Dec 28, 2016)

Normally best to make sure to have the eggs in hand, before counting the chicks, then these eggs will also have to hatch before anyone can cash in on the chickens.


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## rickbb (Dec 29, 2016)

Two other diddies come to mind.

"A bird in the hand is worth two in the bush."

And;

"No one ever went broke taking a profit today, plenty of people go broke waiting for a better deal tomorrow."


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