Aqua Regia Mess -help!

[JustMe]

I'm still trying to figure out why one would attempt gold recovery from heavy sand concentrate with AR. I know it can be done with success, but for me smelting is much easier. Later refining, if desired, seems more straightforward, with fewer complications.

Because of the nature of the tone in this thread, I will not name my site. However, suffice it to say that I have developed a device which recovers gold much finer than people are used to dealing with, in significant enough quantity to be economically important. Generally the gold is recovered from placers, but some people using the device have hard rock mines.

Some of these people, although praising my device, have come to me asking "but how do we get the ultra fine gold out now?..."

I am trying to find an easy way for people to separate this ultra-fine gold without using mercury. Standard mechanical methods do not work well.

I have been fairly successful at simply eliminating as much iron as possible from the sands, roasting off the sulfides and using vinegar and drug store generic hydrogen peroxide to eliminate any lead. AR then seems usually to work quite well. All simple steps without much inherent dangers. If they will at least follow standard acid handling precautions and do the work in the great outdoors in a safe location.

Or do you prefer that I suggest they use:
Mercury
Cyanide
or buy a furnace, crucibles, tongs, flux, etc., THEN smelt and THEN use AR (and inquartation most likely)

Simplest option is for them to send it in and pay to have it recovered. But there seems to be a perception among many that a lot of refiners are not honest and will steal their gold.

Trivia note: The word boil, boils, boiled, etc, is used hundreds of times in CM Hoke's book.

 

[Geo]

it seems to me like this has happened before. JustMe, are you a former member? its a weird coincident that another new member would lay into Harold like that when there were much easier targets to take on. it seems that Harold was baited into making his presence known, and then, JustMe ambushes him and tears into him like it is something personal.

for any new member following this thread, Harold and any other moderator has put in his time here and deserves respect from the members because they gave their time with no gain to share their knowledge. helping to keep us safe, instructing us on how to do the things we love so much. when another members attacks one of the moderators, it should be insulting to all of us equally. unless some proof is offered up front for all to see, any accusations should be treated as rumor and dismissed just as quickly.

 

[solar_plasma]

Justme.....do you sometimes feel like:

characterized by unwarranted feelings of self-importance. They have a sense of entitlement and demonstrate grandiosity in their beliefs and behavior. They have a strong need for admiration, but lack feelings of empathy for others. These qualities are usually defenses against a deep feeling of inferiority and of being unloved. (wikipedia)

??

If this should be your problem, and I say if....then nobody here can help you and you will not find, what you are looking for. And if you find, what you are looking for, you will still not feel better.

 

[JustMe]

it seems to me like this has happened before. JustMe, are you a former member? its a weird coincident that another new member would lay into Harold like that when there were much easier targets to take on. it seems that Harold was baited into making his presence known, and then, JustMe ambushes him and tears into him like it is something personal.

for any new member following this thread, Harold and any other moderator has put in his time here and deserves respect from the members because they gave their time with no gain to share their knowledge. helping to keep us safe, instructing us on how to do the things we love so much. when another members attacks one of the moderators, it should be insulting to all of us equally. unless some proof is offered up front for all to see, any accusations should be treated as rumor and dismissed just as quickly.

Not even going to respond to this gibberish. You are more than welcome to remove my account. Good-day gentlemen.

 

[butcher]

Sigh,
I would not delete this thread, as it does show you do not know what you are talking about, you do not have much knowledge in the processes you attempted, it also shows that you believe you know things you do not, while it does sound like you have learned a little about the processes, you do not understand them well enough to be successful, You make a big mess that anyone who has studied Hokes book would not have made in the first place, then ask for help, when you get suggestions that could help you, you begin to get argumentative, and begin attacking members, when you are brought to light on this, you begin to attack on of the forums most knowledgeable member who could give you the best advice, it does sound like you have maybe been banned from this forum before, if so probably for this same behavior.

Your attitude and attack on Harold has sealed it for me You will be banned from this forum, not only do you not wish to learn, you are just creating trouble here, on this forum.

P.S. read Hoke’s book again, you do not know what it say’s, she did not boil solutions she evaporated, yes she used the word boil, but she used a steam bath heat source that could not reach a temperature that would boil the solution, in fact she even warns against boiling the solution, read the chapter about losses and why you should not boil a solution (page 227) is one example in her book.

 

[eeTHr]

it seems to me like this has happened before. JustMe, are you a former member? its a weird coincident that another new member would lay into Harold like that when there were much easier targets to take on. it seems that Harold was baited into making his presence known, and then, JustMe ambushes him and tears into him like it is something personal.

Now that you mention it, there are a couple former members with similar MOs, that I can think of.

One was, I think, a couple years ago. He would come on like he was a super chemist, suggesting various kinds of "new" processes which he at first claimed to be wonderful. Then when it was pointed out to him, by some of the more experienced members here, that even if his suggested processes worked, that they were way over-consuming of time and materials to do them. And there were also several safety hazards with his suggestions.

He then backpeddled to the position that he wasn't trying to find better processes, but just experimenting to see what was technically possible.

Soon it was discovered that there were parts of his test "proofs" that could not have actually succeeded. It became apparent that he was not actually doing the processes which he was describing, but rather was merely theorizing, either with good intent or not, and yet stating that he had actually performed them and stating their imagined results.

Number two was last year or so. He claimed to be a doctor, I think.

Anyone please correct me if I am wrong about these two, but I think they were both eventually banned, after much commotion among board members.

Do either of these personas seem similar to the subject user?

 

[Palladium]

You know we try and not be judgmental here on the forum regardless of how it may look, but damed if folks ain't making it hard.

 

[NobleMetalWorks]

If you do not understand how to use BDG properly, you have no business using it. Why you thought after using BDG you would be able to precipitate anything from your solution is beyond me.

If you successfully extracted Au from your Ar solution using BDG, but did not wash your pregnant BDG, you might not see a full reduction of Au by Oxalic Acid. This is a step I find many people skip or ignore all together when using BDG. BDG will collect other impurities, these other impurities are easy to remove but must be removed before you attempt an oxalic acid reduction.

In your pregnant AR solution you should be adding 2-3 times the amount of AR solution, again in DI water. After adding the correct amount of BDG you should agitate for at least 1 minute. After agitation, pour into a separatory funnel and allow the BDG to accumulate on the top of the solution, you should be left with a solution of AR on the bottom that is now barren, and BDG which will be gold in color unless it has carried over a lot of other impurities from your AR solution. I have seen the color range from gold, to light green but have been told that some people see other color. In any case your BDG needs to be washed now. I know that sounds strange, but in order to get a good oxalic acid reduction, you should remove all other impurities from the pregnant BDG solution.

I do this by mixing a 50/50 solution of HCl and DI water. Add the solution of HCl into the BDG and again agitate. Pour through a separatory funnel again and allow the BDG to once again separate from the HCl solution, you will now notice that some color has transferred from the BDG to the HCl. These are the other impurities that carried over into the BDG when you agitated it with your AR solution. Retain this, and test for values accordingly.

Your pregnant BDG solution should now be gold in color, if there is still other color wash again with your HCl solution until it is gold in color.

Heat the BDG but DO NOT BOIL, heat the Oxalic Acid you dissolved in DI water, but again DO NOT BOIL. Try to keep both at the same temperature, once all the Oxalic acid is dissolved, slowly pour into the pregnant BDG solution and again keep on heat, but DO NOT BOIL. Using a stir bar is a good way to insure you are getting good exposure, if you do not stir the solution the gold will reduce between the BDG layer and the Oxalic Acid solution and stay there. Precipitation will start almost Immediately but can take several hours to complete.

The important thing here is to wash your pregnant BDG solution with a solution of HCl, and to agitate while reducing the Au from BDG, and to keep the solution on heat, but not to boil.

Scott

Edited, there seems to be a lot of mis-information about BDG in this thread.

The odd thing is that I can not find the butyl diglyme upper phase, even now that I have eliminated most of the liquid. It's possible that it has evaporated, but I'm not certain of that. I don't know offhand what it's vapor pressure is.

I have been using BDG to good effect, and have not yet encountered any evaporation, but I don't think a pregnant solution of BDG would do so anyway. It's an oil based solvent, this is the reason it floats, and it is not very soluble in water, I see very little loss and use it over and over.

Yes, I heated the oxalic acid and the aqua regia solution. I attempted to use copper to cement it all out and it did nothing. There was no reaction. I added a small amount of zinc powder to the solution, and it appears to have worked, and now the stannous test shows only a slight coloration change when added instead of a dark inky purple-black look so most of the gold is now out of solution.

I'm a little confused at this point, are you saying that you had BDG in solution, then added oxalic acid to the BDG/AR solution? Before you add Oxalic Acid to BDG, you have to separate the BDG from the AR solution, clean it, and then heat it, add the heated oxalic acid solution, etc. If you had BDG in an AR solution and then attempted to cement out the Au with Cu, it would do NOTHING because the Au would be in your now pregnant BDG which should be floating around on top somewhere.

Not sure how to go about removing the BDG at this point. Now I do see an upper phase which amounts to a few oily looking patches on the surface of the solution. Certainly nowhere near the original 30ml I began with. Maybe just a couple ml now. I suppose I can soak it up with a cotton ball and discard that way.

If you soaked up your BDG that was floating around on the top of your solution, and threw the cotton swabs away, you just discarded your Au. BDG does a wonderful job of extracting Au from AuCl solutions, even if dirty.

I searched Hoke's book, 365 pages and found nothing about Butyl Diglyme, or Butyl Carbitol or Diethylene Glycol Butyl Ether, etc.

You are not going to find anything in Hoke's book on BDG, it wasn't even discovered to be effective in extracting Au from AuCl until the 90s I believe. Hoke was long dead and buried before BDG was ever used. BDG is an organic solvent, Hoke deals with Inorganic Chemistry, not Organic Chemistry.

Update on what's going on here:
BDG is gone now. Tested the solution several times after adding the zinc powder and it was virtually free of gold.
Used a buchner filter, and re-tested the liquid which is now a nice lime to light emerald green (used to be a deep golden yellow). The liquid tests positive for a lot of gold, but prior to filtering it was free of gold for the most part.

But at least now the BDG is gone and the sediments are gone. Now maybe I can get somewhere.
Sulfuric acid now and boil it down?

If you had a solution with BDG, and removed the BDG, dropped everything lower on the reactivity scale with Zinc Powder, you would have NOTHING in solution. Not only that, but whatever powder you dropped with Zinc, would have NO Au, you threw your Au out, whatever there might have been, with your BDG.

Have you tested your Stannous Chloride against a known standard solution of AgCl? Because if you did not, it seems your Stannous Chloride is giving you false indications.

Black sands were processed. Magnetics were removed with rare earth magnet. Hydrochloric acid used to dissolve away additional materials. Roasted to remove sulfides.

You should roast prior to using any acids!

Remaining sands were placed in a beaker and nitric acid and hydrochloric added in a ratio of 3:1.

You should be making small additions of HNO3, not making up a solution at 3:1. If you didn't roast before using HCl, you could have all kinds of things going on, then if you made up a mixture of Ar according to 3:1, you possibly could have used up all the HNO3 in secondary reactions before ever dissolving any Au that may have been present. When you have an excess of HNO3, your secondary reactions burn the HNO3 faster than if you made small additions over a period of time. As well, you would have added enough HNO3 to dissolve whatever metals you had in your material, and not needed the Urea later.

Was let set for a few hours. Liquid was filtered then put into a separatory funnel. 30 ml of BDG were added and it was shaken vigorously for several minutes, and allowed to sit. Upper phase never showed up.

You should have added 2-3 times the amount of AR solution, in DI water, If the solution was shaken vigorously for several minutes in an AR solution that was no diluted, and contained Urea, and the BDG was fractionated into small beads of oily solvent, the thick solution that has a totally different PH than what normally it should, would take an extended length of time to accumulate and float to the top. You simply didn't wait long enough.

I decided to separate the top portion anyhow, feeling that maybe it's coloration was too similar and index of refraction too similar to see easily. .

The BDG is an oily solvent, you can plainly see when it separates. Just as easy as you can see oil in water.

Then took the top 30ml or so and put in a separate beaker, mixed oxalic acid in distilled water and heated, and heated the AR as well and mixed the two

You didn't remove any BDG unless it was a very small amount, you didn't wash the pregnant BDG, you added your Oxalic Acid solution into your AR which is not going to reduce any Au in your solution because you only have, if any, a very small amount of BDG in your 30 ml of AR solution. Not only that, but by adding your Oxalic Acid solution to your AR solution you have diluted it's effectiveness.

No precipitation. Let set for a few days to see if separation would happen and it did not either in the top liquid I added the oxalic acid to or the bulk of the liquid that was set aside. That's when I put it on the shelf for later study.

That I might make some explosives with nitric in solution which is GONE because it has been evaporated off because people 'helping' here are not reading what I wrote.

Yeah, you don't have anymore HNO3 left, and could have converted SOME of it to Urea Nitrate, which is not something you want to be doing. If you did make Urea Nitrate, you wouldn't have any free HNO3 left, duh...

Oh and I solved the issue but I bet you guys knew all along that that film on the glassware was causing the issue ... right? So what exotic film that might be almost imperceptible on glassware might cause this to happen AND affect butyl diglyme.

I think your failure with BDG lies strictly with how you used it, not in how it might have reacted to any minute amounts of some exotic film not cleaned off your lab glass, that you seem unwilling to express what it might have been. If you claim it was unknown I will loose what little respect I may have had for you. Arguing your point while pointing a finger at an "unknown" is not factual evidence, is not empirical data, is not good chemistry and certainly not good science. I'm going to stop right here I have heard enough. You are either outright misleading people because you are embarrassed by what other people consider mistakes that could be easily avoided, or utterly without the experience and self education required to be using the methods you have mentioned. You should not be assaying by dissolving material into any solution, you should be assaying properly. You shouldn't be using BDG because it's painfully obvious that you have no clue how it's suppose to be used. You should be processing your material correctly, not digesting in acid, then roasting, that makes no sense. You shouldn't be adding unknown results with unknown results and then adding more to create complex solutions, specially when you have no clue about the potential risks in doing so, SPECIALLY when you could be unknowingly creating volatile and explosive solutions.

I cannot even imagine a situation where you would feel justified for people pointing out your mistakes, and not giving you the answers you are looking for. Not when you have not been clear about what exactly you have done, or how you have done it, and it's painfully obvious that you are not processing material correctly, and combining things you shouldn't be. You want someone to hold your hand and tell you what to do, and expect them to guide you, when you don't even know how to properly conduct yourself on this forum, nor how to properly process the material you are attempting to.

BDG works amazingly well, but before you go skipping off to attempt using BDG again, I would suggest learning a lot more about the more common ways of processing material. Educate yourself so you can effectively communicate with people on this forum.

I'm disgusted

Scott

 

[its-all-a-lie]

it seems to me like this has happened before. JustMe, are you a former member? its a weird coincident that another new member would lay into Harold like that when there were much easier targets to take on. it seems that Harold was baited into making his presence known, and then, JustMe ambushes him and tears into him like it is something personal.

for any new member following this thread, Harold and any other moderator has put in his time here and deserves respect from the members because they gave their time with no gain to share their knowledge. helping to keep us safe, instructing us on how to do the things we love so much. when another members attacks one of the moderators, it should be insulting to all of us equally. unless some proof is offered up front for all to see, any accusations should be treated as rumor and dismissed just as quickly.

Not even going to respond to this gibberish. You are more than welcome to remove my account. Good-day gentlemen.

What happened here? The definition of respond is as follows:

re·spond
/riˈspänd/
Verb: Say something in reply.
Noun: A half-pillar or half-pier attached to a wall to support an arch, esp. at the end of an arcade.
Synonyms
verb. answer - reply - react - rejoin - return
noun. response - reply - answer - replication - rejoinder

 

[JHS]

Hello,
This is exactly what makes the search so hard to
find the information that is required to further
one's education on the subject of this discussion.
one page of value,and two pages of soap opera.
name calling is not part of refining.
I AGREE THAT HAROLD WAS CORRECT IN CORRECTING BOILING.
HE SHOULD NOT HAVE BEEN ATTACKED FOR THIS.
But the rest of all the non esental comments, makes it that much harder to
find the information we seek

john

 

[Harold_V]

Needless to say, I'm late getting back to this post, which has been handled more than adequately by other readers and our trusted moderator, butcher. Still, I have comments to add.

I have been reading these forums for years, and have searched your site many many times. I have a copy of Hoke. In all that time, I had never needed to post here. I am fully aware of how you work Harold. I have seen it over and over in numerous posts on your site.

Interesting, but the facts betray your claim. If you had been reading for years, you'd know this is NOT my site, nor do I lead anyone to believe it may be. I am but a moderator on this board, assigned to ensure that it operates without problems.

It is unlikely that you will allow this thread to remain, since rather than slink away as you preferred, I make this post.

If you had the slightest idea of what I expected, you'd know that I would not delete this thread, nor should it be deleted, as it stands as a perfect example of how new readers should not behave---assuming they have any hopes of remaining on the board, which operates exceedingly well without the likes of you, and has for many years. You, sir, are akin to a mindless child in junior high school, proven through your posting on a subject about which you know very little, and lack the wisdom to be advised by those who do. As for slinking away, only you can determine if this board has value to you, or not. Wise individuals who hope to learn quickly understand that this board, unlike the vast majority of them on the internet, does not tolerate rudeness, nor do we allow misinformation to stand. We expect that if a new reader hopes to profit by the ability to post here, that said reader will be on his best behavior and appreciative of those who spend their valuable time trying to assist others. Clearly, none of that is shown in your responses.

Does anyone need to be reminded that being on this board is not a right? It is a privilege extended to you by the rightful owner, and it is my job to ensure that that privilege is not abused. It is a job I take seriously, as if the owner was my own son.

I take offense at being made a fool publicly, or used as an unwilling example fitting into your private agenda or the brunt of a thinly veiled insult.['quote]
Then you should have considered the old addage, "it is better to be though a fool than to open one's mouth and remove all doubt". You, sir, are a fool.

It's called being a man Harold, sometimes we do have to stand up and be a man. If you wished to use my posts to set examples for others, you might have consulted me and asked if I could help you to do that and was willing to play along for the benefit to others.

We do not beg readers to cooperate. If they cherish their presence on this board, they willingly cooperate. What they don't do is "stand up like a man", which is a sure sign of your childish mind. You have chosen your ego over your opportunity to be a member of this board. Not a problem. We've dismissed many like you, and I expect many more will, likewise, be dismissed. The board is better for your discharge, and our life goes on. You, by sharp contrast, can seek information (or display your lack of knowledge) elsewhere. However, you'll come to understand that you have just killed the goose that lays the golden eggs, as there is no other source of reliable information at your disposal. You won the battle, but you lost the war.

This entire thread is unlikely to remain, so I have taken screenshots of the entire thread and will most likely post it on my mining related site with an interesting discussion of it there at some future date. There is something to be learned here.

Yes, there is something to be learned here, but I expect you'll not learn the lesson. Your type never does.
Screen shots are of no value, as this thread will remain, and it will remain without being edited. We have nothing to hide, nor anything for which we owe an apology. It is you, sir, who is out of line, which will become clear in the future.

It never ceases to amaze me how far some folks will go out of their way to ruin what is a good thing for themselves, all in the name of ego. Had this individual done some listening instead of endlessly running his mouth, he would have been rewarded with considerable assistance. Instead, he chose to rebuild the forum to one of his choosing. To that end, we, here, do not permit the monkeys to run the zoo.

Harold

 

[Harold_V]

Hello,
This is exactly what makes the search so hard to
find the information that is required to further
one's education on the subject of this discussion.
one page of value,and two pages of soap opera.
name calling is not part of refining.
I AGREE THAT HAROLD WAS CORRECT IN CORRECTING BOILING.
HE SHOULD NOT HAVE BEEN ATTACKED FOR THIS.
But the rest of all the non esental comments, makes it that much harder to
find the information we seek

john

And it's the reason why we ban readers who do not heel. We have a strong policy on this board of not permitting behavior that causes disruptions. When a reader is corrected, the only acceptable response is one of cooperation. If that isn't forthcoming, you can assume the responsible party will be banned, as has been the case.

Harold

 

[Harold_V]

Because of the nature of the tone in this thread, I will not name my site. However, suffice it to say that I have developed a device which recovers gold much finer than people are used to dealing with, in significant enough quantity to be economically important.

Right! You, who hasn't enough sense to not use AR for processing an ore, has developed a revolutionary device to extract gold when tens of thousands who have gone before you were not successful.

I expect that device is akin to your web site. All in your mind. And you hope to punish us by not allowing us access! My, my, my, what will we do?

Harold

 

[solar_plasma]

JHS wrote:Hello,
This is exactly what makes the search so hard to
find the information that is required to further
one's education on the subject of this discussion.
one page of value,and two pages of soap opera.
name calling is not part of refining.

Whenever more than 2 persons interact, you will likely see 3/4 of the time soap opera: forming, storming, norming, performing. When you work together with people you know and have worked with before, the forming of the team, the storming who are they, who is me, what do we talk about, where do we stand and the constitution of norms are already done and you are mostly in the state of stable performing.

I would say, this is almost not possible on a living forum with new members all the time. But the fact is, the soap opera itself has brought up some goldnuggets like among others noblemetal's long explaination of what went wrong in the process, something worth printing and put into the chapter about BDG. Also The way the mods and merited old members communicate and handle social problems and their rhetoric contains some goldnuggets, I at least learn from.

I agree, the soap operas make it hard to find the goldnuggets afterwards, but isn't it that what goldnuggets a priori are, - hard to find?

 

[Geo]

My solution to the problem:
I dried the mixture out and then added BDG directly to it, capturing the auric chloride, put it through a filter to remove the particulate matter and then dropped out the gold as powder using hot oxalic acid (also having heated the BDG. I left out a few of the other obvious steps too.)

for anyone still interested on why he failed with his recovery, its in this quote. he dried the solution completely and then added the BDG. i had to read the entire thread again to see if i could find some very obvious mistake that would account for the loss of the BDG and its inability to capture the gold. he added the BDG to a dry mixture and then poured that through a filter. he will never be accused of being too intelligent.

goodbye to bad rubbish.

 

[Platdigger]

I agree solar_plasma, NobleMetalWorks post about BDG makes this thread more than worth it.

 

[JHS]

Update on what's going on here:
BDG is gone now. Tested the solution several times after adding the zinc powder and it was virtually free of gold.
Used a buchner filter, and re-tested the liquid which is now a nice lime to light emerald green (used to be a deep golden yellow). The liquid tests positive for a lot of gold, but prior to filtering it was free of gold for the most part.

But at least now the BDG is gone and the sediments are gone. Now maybe I can get somewhere.
Sulfuric acid now and boil it down?Top Report this postReply with quote

why would the solution change to green?
If BDG lockes the gold in its matrix,how could removing the BDG allow the solution to test posative?
just trying to learn and understand.
john

 

[NobleMetalWorks]

why would the solution change to green?
If BDG lockes the gold in its matrix,how could removing the BDG allow the solution to test posative?
just trying to learn and understand.
john

It's really difficult to understand how the OP came to any of the conclusions he did, or produce any of the results because frankly, some of them are impossible.

However, if the solution was gold in color prior to whatever else he did, and he removed the BDG and the solution is now emerald green, it could be he removed the Au with the BDG, and is left with a solution of other metals like Cu for example, that would color the solution green.

Some people associate the color green with Au, but that's only because so much of the material that is processed has Cu associated with it.

He might have picked up on that somewhere on another post, and assumed it meant Au. It's obvious that he didn't test properly with Stannous Chloride, it's also obvious he didn't have a standard solution to test again, and it's further obvious that he either did not do what he said, and stated his process incorrectly on this thread, or is outright lying.

As a reader you can snip away 99% of what he said, just leave his name and that would be the only value in everything he has posted, in this particular thread, other than a good solid lesson in what NOT to do, and what NOT to post, and what attitude is not accepted by the moderators.

After I got half way through his posts about what he did, and BDG, etc. I finally decided that it wasn't worth attempting to make sense of what he posted because it just simply wasn't possible for him to do what he claims he did.

Scott

 

[eeTHr]

I also noticed that there are several places in his posts, like the use of "boiling," which strongly contradict his claim of having read this forum for a number of years. I still think that he may have been one, or both, of the two previous member that I mentioned above. But who knows? 8)

 

[Harold_V]

If he's an ex reader, he has a new ISP.
He thought himself clever in not disclosing who he was, but all individuals who post leave behind their identity. He's from Arizona, a known hot spot for scammers.

Back in the late 1900's, one of the common scams to come from that area was the discussion of gold ore that was exceedingly high in content, but would not fire assay. It was reported that the gold was there, but it was "immature"--not yet fully formed as gold.

Oh, hell yeah! That happens all the time.

Anyone want to buy a bridge? I have a nice one for sale. Stone. Used to be in London.

Harold