Aqua Regia Mess -help!

[JustMe]

(snip)
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.

Communication is a 2 part process. One initiates a communication the other perceives it. Requiring people to phrase things properly may be important in chemistry, in which I would agree.
(snip)

As a correction to your wrong assumption on the "Nitric", it is still their.
Only the ""excess"" nitric was removed by "evaporation", which means my earlier post is still correct. If you had a decent understanding of "Chemistry" you would know this, Hence my pointing it out for those who don't know.
It will remain in solution even after you have dropped the gold with your precipitant of choice, so keep any cotton products away from any solution that has ever contained nitric acid.

This follow up post is for those who come later and might try to follow your mistaken knowledge.

I know how to make nitrocellulose and have. Nitrocellulose is not a primary explosive and requires a spark or flame or some other external cause to detonate. Nitrocellulose is sold as flash paper and lacquer for guitars. You might also note that the original 'failed' experiment with BDG contained 30ml of BDG of which later I stated that a few ml of BDG had appeared after the zinc was added. I also said I mopped it up using some cotton swabs (7 to be exact), and I used capillary action to suck the bdg off the solution and likely got none or extremely little on the qtip at all. So if you would like to make a general statement to others reading the thread regarding the safety of using cotton with nitric acid containing solutions, do it. But don't make it sound like I just made a batch of high explosives here that my neighbors (which I don't have) should be concerned about! With as much potential nitrocellulose as could possibly be made with the cotton on 7 qtips if it had all been converted, I would be lucky to blow up a plastic zip lock bag with it!

A potential fulminate product would be a much more serious consequence of all this. Fulminating gold anyone??

 

[JustMe]

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.)

Just to make sure I didn't get anything but gold, I re-dissolved it with AR and re-precipitated it with SMB.

Recovery was 2.3gm of heavy shiny yellow stuff, happily, quite a bit more than I expected.

Thanks for your help. It was the statement of the obvious (well obvious to me anyhow) that I was overlooking. "... if you have gold in solution, its not going anywhere until you do something. it wont evaporate away." ... but like the nitrates, it's not gold ... it's chloride of gold. Auric chloride, the thing that BDG has such an affinity for.

 

[Platdigger]

Just a few things of note. First off congrats for recovering the gold from this mess of chems!
One is I have not heard of adding BDG to dried salts like you did, nice.
Also I am curious if you instead of using urea and by evaporating down a few times if the ferrous sulfate would have worked at the beginning of this.
The last being that, that was a good find about the BDG somehow not working because of some type of film on (in) the glassware. I think this may have been stated on the forum (by Steve I believe) but is good to be reminded of.

Oh and, one of the reasons some of the responses to your posts may have seemed harsh is the fact that this forum has had "AR mess-Help!" type of threads posted here soo many times. And usually by folk that do not have a clue to what they are doing.

 

[JustMe]

Ferrous sulfate was used in one of the three failed batches that got mixed up in this mess. I am sure there was some excess in that batch and adding to the rest of the mess and evaporating down did not precipitate anything. Urea and SMB was used in only one batch. And BDG and oxalic acid was used in only one batch. Ferrous sulfate the third. After letting the evaporated solution sit a day, I mechanically removed all the crystalline solids that i found in it.

I didn't want to add more ferrous sulfate as it had already failed me once in the mess and I was convinced that it was some complex ore chemistry that was causing all the problems. In a way it was. That film was from some OTHER ore and chems that were used to extract a different type of metal, that is a bit exotic (well at least for me).

 

[butcher]

JustMe,
You keep asking where you went wrong, and wanting us to point them out, where do we start, it sounds like you combined 3 problems into one big mess You keep getting the answer to read Hoke's...
I see several things that were done wrong, but it would do you no good to try and point them out, at this point you needed to try and get the gold out of this solution safely, and get it melted into metal, then you can spend the time needed to study to learn to do these processes right.

I think you can see where you made most of your mistakes, by studying and practicing what your learning you will learn better methods and you will not make these same mistakes.

 

[JustMe]

JustMe,
You keep asking where you went wrong, and wanting us to point them out, where do we start, it sounds like you combined 3 problems into one big mess You keep getting the answer to read Hoke's...
I see several things that were done wrong, but it would do you no good to try and point them out, at this point you needed to try and get the gold out of this solution safely, and get it melted into metal, then you can spend the time needed to study to learn to do these processes right.

I think you can see where you made most of your mistakes, by studying and practicing what your learning you will learn better methods and you will not make these same mistakes.

*sigh* ... did you happen to notice that I have solved the problem AND already got the gold melted down into a cute little nugget?
I think a few of those "where did I go wrongs" were rhetorical. No?

Did you happen to notice that I made mention of the fact that people were giving advice without reading all I wrote first and that that can be as dangerous as anything I might have done/do? Especially if they missed the fact that I mixed anhydrous ammonia with the stuff before I dried it out?? Any alarms go off when you told me to smash all the dry stuff up with a hammer to make sure it's good and powderized?

NOO NOOO! I DIDN'T. Was just to make you look.

Did you happen to notice that I knew it was a mistake and that I did it simply because I got p***** off and didn't think first?

OH, NOW THERE IS A LESSON! NEVER MIX CHEMICALS WHEN YOU ARE P***** OFF AS IT CAN BE VERY DANGEROUS!

 

[solar_plasma]

I am glad you solved your poblem. I did not read the whole thread again and can't remember all of it. But I think I know, what happened here between the lines.

You wrote:

Ferrous Sulfate did not require neutralization of the nitric

in one of your first sentences. Using the word neutralization is not correct, even misleading, which shows, we at this point do not use the same language. The mods often pointed out, that reading Hoke also important to establish a set of terms and concepts that is common to all and everyone understand it the same way. I you are repairing the breaks on your car, you willl be able to so, even if you call your brakes "Otto", but talking about repairing your "Otto's" nobody will understand you.

Even worse, people get easily the impression, that you don't have a clue and then they react like to someone, who is a danger for himself and others. Esp0ecially, when your description is loaded with different methods used in one process.

This may be an example to all of us: Use (and learn) the right and proper terms.

 

[butcher]

I did read this:
"I re-dissolved it with AR and re-precipitated it with SMB.
Recovery was 2.3gm of heavy shiny yellow stuff, happily, quite a bit more than I expected.

They way I read it you had some heavy yellow shiny stuff, so I assumed you had gold or a yellow powder, salt, or something that was yellow.

I do not see where you have solved any of the problems, even if you recovered gold from this batch, as many of your problems came from not having a good understanding of the recovery process and the refining processes, these were where the problems began, and what we have been trying to help you with, by telling you to study Hokes book and read more of the forum.

I did not see where people were trying to help you, and give advice without reading.

I sense you do not like hearing the advice, and think you know better, which it is obvious to me you think you know more than you do, so my main advice for you is to spend more time learning better procedures for processing.

Why would anyone ask for advice then not want to accept the advice given, thinking they know more and do not need it, or to bite back at those trying to help? If you already know more than they do why would you need to ask for help, if the suggestion for help were not suited to your problem or the advice was off, why not just say thank you.

I do not find your jokes or attitude on the safety funny, you had many different chemicals in that mix, speaking of ammonia (urea can break down to ammonia), and with all of those chemicals mixed up, there is not much telling of how dangerous that mix could have become, or in what conditions it may have become dangerous.

Not only is it dangerous to mix chemicals with a bad attitude, but that attitude here on the forum makes it harder to learn from those trying to help you, and it can also cause a member who has a chance to learn from others here, to lose that right.

JustMe, I am glad you got that gold back safely, and hope you understand how to treat your waste, if not we have a good thread on that in the safety section "dealing with waste".
I also hope you lose what seems to me to be an attitude, and join us in our search to learn more, we all make mistakes, and non of us know it all, and we can all help each other to learn more.

 

[solar_plasma]

I consider it as essential never to swap from one method to another. When the choosen precitpitation method not is working, then there is a reason for it. This reason has to be solved or we should go over to clean up the mess. Recover the values and start again at the beginning. It is not only in refining the fact, that focusing on the problems and trying to fix them with fix ideas, just create new problems, that even may be harder to solve. I have learned in my short time, and you may correct me, there is only one method of choice, which leaves no space for trial and error. Doesn't it work, go back to the start.

 

[Geo]

getting my values from solution was never really a problem for me. aside from months spent studying on the process i intended to try, i knew that no matter what i did to get the metal into solution, i could always cement the values out with copper if my preferred method didnt work. too much free nitric or too much heat or not enough heat, too much chlorine or bad SMB. it didnt matter, i knew that with a little time and patience, i would still get my gold. in the words of Kevin James "why sweat the small stuff"?

 

[JustMe]

I did read this:
"I re-dissolved it with AR and re-precipitated it with SMB.
Recovery was 2.3gm of heavy shiny yellow stuff, happily, quite a bit more than I expected.

They way I read it you had some heavy yellow shiny stuff, so I assumed ...*snip*

I do not see where you have solved any of the problems, even if you recovered gold from this batch, as many of your problems came from not having a good understanding of the recovery process and the refining processes, these were where the problems began, and what we have been trying to help you with, by telling you to study Hokes book and read more of the forum.

I did not see where people were trying to help you, and give advice without reading.

I sense you do not like hearing the advice, and think you know better, which it is obvious to me you think you know more than you do, so my main advice for you is to spend more time learning better procedures for processing.

Why would anyone ask for advice then not want to accept the advice given, thinking they know more and do not need it, or to bite back at those trying to help? If you already know more than they do why would you need to ask for help, if the suggestion for help were not suited to your problem or the advice was off, why not just say thank you.

I do not find your jokes or attitude on the safety funny, you had many different chemicals in that mix, speaking of ammonia (urea can break down to ammonia), and with all of those chemicals mixed up, there is not much telling of how dangerous that mix could have become, or in what conditions it may have become dangerous.

Not only is it dangerous to mix chemicals with a bad attitude, but that attitude here on the forum makes it harder to learn from those trying to help you, and it can also cause a member who has a chance to learn from others here, to lose that right.

JustMe, I am glad you got that gold back safely, and hope you understand how to treat your waste, if not we have a good thread on that in the safety section "dealing with waste".
I also hope you lose what seems to me to be an attitude, and join us in our search to learn more, we all make mistakes, and non of us know it all, and we can all help each other to learn more.

Ok one last attempt to explain my position:

There are no 'ratings' that I can see here as to how 'expert' of advice I am getting from a member. One of you could be the world's foremost chemists with a nobel prize under your belt. Another could be a whack job from New Jersey who just happens to know how to speak chemicalese. And another could be a malicious person intent on teaching lessons to idiots.

So if you are right and I know nothing, and you wanted to help me, it would seem that allowing ME to choose amongst a set of solutions provided by varying degrees of expert advice, could be dangerous. After all, who am I to judge who here is best suited to advise me and the 'most right' on how to go about the fix for the problem I presented, especially if I know nothing as you suggest.

And multiple solutions were presented.

One solution offered was to introduce sulfuric acid to the concoction, one was to read Hokes book, (which in itself could have been a problem because I might still not have understood the solution given in the book if in fact I am such a novice), and another was to cement it down using copper. I tried copper and it did nothing. No answer was ever given to my question about using zinc, and that ended up being what worked instead of copper to cement the solution down.

And as I stated before, the problem appears to have been due to a film on the glassware, not the processes I used. How did I find that film? I kept trying to see if I could see an upper phase using all kinds of different lights and lighting angle, and finally noticed above the solution line a silverish-tanish-yet-clear looking coating on the glass. Since fully cleaning the glassware, I have successfully repeated all 3 processes, and all have been successful. (They were 3 separate batches that ended being mixed together, not one that I kept using different chemicals trying to get the gold out of like Solar seems to think).

The glassware had been used in a process of separating Nb from a complex ore. And a few custom chemical approaches to simplify it's removal, one of which was cyclohexanone (yes I know that is used commonly for that purpose, I meant that it was one of the chemicals used and probably what was in the film that may have helped cause the problem with the BDG, not the novel approach I was attempting. And although intriquing, I simply don't have the time to sort out what exactly that film was that did this or if it was the alignment of the moon and jupiter)...

I was not the only one to joke, and it's true, some people do not have a sense of humor.

 

[Geo]

JustMe, have you ever heard of a "stock pot"? if you read Hoke's book, you would have. a stock pot is a container that you place all of your spent solutions you have precipitated from. believe it or not, you cant get it all on the first go around. this pot is a mixture of just about everything or at least everything you have worked on. its a big mess of chemicals and compounds. Hoke teaches us how to use and finally recover values from the stock pot that would have been tossed out otherwise.

what you were dealing with may resemble what might come from a stock pot. a mix of all the chemicals you worked with that still contained values. gold chloride is acidic and will cement out of solution on copper. it may have been slow because of everything mixed with it but it will cement out. notice where i said "with patience" before. it takes time. sometimes weeks to cement all the values out of solution. if you dont see an immediate reaction doesnt mean that its not happening. when you tried to cement on copper, did you heat the solution? it makes the reaction speed up.

 

[JustMe]

If it is of any value, the copper immediately turned black AND got an oily coating on it, then the reaction stopped. Obviously the BDG. Not really any way for it to react further. Essentially it was working in a similar fashion to a chelate (that the right word ... preferential wetting?), gold trying to coat the copper, pulling the BDG with it and covering the surface of the copper, keeping any further solution from coming in contact with it. Did I get that wrong?

At least to me when I saw it happen, it was fairly clear what was going on.

The solution was hot (about 85C if I recall).

Yes, I have heard of a stock pot. My 'problem' and it's similarity to a stock pot somehow didn't make connection in my brain for some reason though.

 

[Geo]

then you had the answer to your problem all along. BDG is an organic compound. by evaporating to a syrup after adding sulfuric acid would have removed the BDG from the mix. re-hydrating with hcl would have left you a cleaner solution to work with. BDG is messy and oily and should never be used in equipment used for other processes. lesson learned on that one. after re-hydrating, the BDG would be carbon and would need to be filtered out before precipitating. preparation of materials is key. knowing what you have in solution is step one, knowing how to deal with them is step two. you knew you had an organic compound in solution so you should have known it had to be removed before precipitating. point is, study the process you are going to attempt, even (especially) if you have done it before and it didnt work right. from the way you described it, you had three failed attempts in a row. did you have any refines that were successful?

the 30 ml's of BDG that you put in the mix should have settled out given enough time. did you filter the solution of all the sand before you mixed the BDG with the solution? this may sound funny but the sand will hold the oil. if you left the sand in the mix, did you put the material in a graduated cylinder and vibrate?

 

[JustMe]

Well, as I stated earlier, the BDG never separated (even after a week) on that (1 of 2) failed trials of a new process.
What was perplexing was the fact that a process I have repeated probably 40 times at least, my normal method of using AR and SMB to recover gold, also failed just prior to the ferrous sulfate attempt and the SMB attempt. I was convinced it was chemistry complexities in the ore sample that was from a different source than normal. After all, ores can have all kinds of stuff in them! I have been lucky for the most part all along, that I have been able to recover gold from black sands and ores using AR without much difficulty prior to this.

And yes ... as I said, 40 successful (without any failures) refines prior, and 3 successful since I cleaned the glassware. The film on the glassware was NOT however BDG.

The balck sand/crushed ore particles had long since been removed from all these batches. There were a few small particles that I got in there, but that was probably contamination that occurred somehow since it's been sitting around in the shop while I pondered my next step. The sand in the solution would have amounted to a few mg.

The filtered clear solution was placed in a separatory funnel, BDG added, and shaken for a few minutes to collect up the gold chloride. It was then left to sit ... and sit ... manifest any emulsions or upper phase. It was as if it just vanished into solution. The original solution was AR, 3parts HCl and 1 part Nitric. So the things that were 'unusual' in that batch were:

New and unknown ore chemistry (sulfides, tellurides, arsenic, etc., possibly in it)
Film on glass discovered later
BDG that was not BDG or perhaps watered down somehow by someone unscrupulous trying to make more profit. Never used BDG before so I am not 100% sure that it was. It's what I paid for and bought and that is what the label on the bottle said, but do I really know it was BDG or 100% BDG? No. If it was somehow diluted down, that could explain that in the end I only had a few ML to soak up and not 30ml. Who knows.

So where did the rest of the BDG go anyhow? - 30ML originally there, sopped up around 2 or 3, nothing left in there now and solution was evaporated down to 150ml or so from 1000ml. No liquid was removed otherwise.

 

[solar_plasma]

Never used BDG before so I am not 100% sure that it was. It's what I paid for and bought and that is what the label on the bottle said, but do I really know it was BDG or 100% BDG?

I think I've read about bad BDG before on the forum. Sorry, if I misunderstood you earlier. It is also my fault, that I didn't see, you have posted under "
Board index ‹ MINING & METAL DETECTING ‹ Prospecting, Mining, Ore Concentrates & Geochemical" and just wondered when you said "minerals". I have no clue about ores and thought, you were processing e-waste. If someone gets such a mess with e-waste, he just do not know, what he is doing.

 

[Harold_V]

Why would anyone ask for advice then not want to accept the advice given, thinking they know more and do not need it, or to bite back at those trying to help?

That's real simple, my worthy friend. He isn't seeking advice, he's seeking endorsement, an attempt to display how *clever* he is. That, in my estimation, is a big mistake. I have little patience with *clever* people.

To JustMe---serious up, and show due respect. Take your attitude far from here, or quietly remove yourself from the board. There will be no further warnings.

What the hell is wrong with some of you guys?

Harold

 

[JustMe]

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

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. 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.

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.

I have already demonstrated here that many people are making assumptions, do not read fully and/or do not understand fully the question asked of them, and do not fully ask the appropriate questions required to get important missing information before giving advice. You're right. Someone will get hurt. You are going to hurt someone. And unfortunately you will blame them and not give it another thought. Also, CM Hoke is not a valid source for safety, either, so perhaps you could focus more attention in the advice you give on that. Tell the fool that he might blow himself up and what to have on hand in case he does!

Harold, as much as you hate to hear it ... you're wrong.

In fact, it might be possible that I did as much or more to contribute to the safety of novices, fools, beginners and others by pointing out the problem that you apparently have overlooked, being myopically focused on terminology and amateur psychiatry.

READ AND UNDERSTAND WHAT YOU ARE GOING TO GIVE ADVICE ON AND IF YOU DON'T HAVE ALL THE INFORMATION OR FACTS, ASK QUESTIONS TO BE SURE YOU GET IT AND ONLY GIVE ADVICE ONLY WHEN YOU ARE SURE. ASSUME NOTHING.

 

[galenrog]

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.

 

[jimdoc]

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.

Any chance of a link to this website? I may want to check it out at some future date.

Jim