Neutralizing Acid

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cfoster78

Member
Joined
Oct 15, 2013
Messages
11
I have a question for the experts here. I have read up as much as I can on the process of gold extraction (including Hoke), and have a degree in Chemical Engineering, so I feel as though I am relatively informed about this process. However, upon attempting it, I have run into a small problem that I am needing assistance on. After dissolving the gold into AR and neutralizing the nitric acid with urea, I began adding the SMB. However, since the urea does not neutralize the HCl in the AR, I end up adding LOTS of SMB which ends up neutralizing the HCL and I can't seem to get the gold to precipitate out. Am I missing a step in the process by not neutralizing the HCl prior to attempting to precipitate the gold, or do I just keep on adding SMB until all of the HCL is neutralized and then continue adding it after neutralization occurs in order to get the gold to precipitate?

Any insight into how I should proceed would be greatly appreciated.
 
cfoster78 said:
I have a question for the experts here. I have read up as much as I can on the process of gold extraction (including Hoke), and have a degree in Chemical Engineering, so I feel as though I am relatively informed about this process. However, upon attempting it, I have run into a small problem that I am needing assistance on. After dissolving the gold into AR and neutralizing the nitric acid with urea, I began adding the SMB. However, since the urea does not neutralize the HCl in the AR, I end up adding LOTS of SMB which ends up neutralizing the HCL and I can't seem to get the gold to precipitate out. Am I missing a step in the process by not neutralizing the HCl prior to attempting to precipitate the gold, or do I just keep on adding SMB until all of the HCL is neutralized and then continue adding it after neutralization occurs in order to get the gold to precipitate?

Any insight into how I should proceed would be greatly appreciated.
My suggestion would be to continue studying. From what you've written, we can see you haven't really "read up as much as [you] can".

You do not neutralize nitric acid with urea. Use it on your garden, but keep it out of your recovery and refining processes.

Excess HCl does not interfere with the precipitation of gold with SMB.

It may take more than a day to assimilate all the information on this forum.

Dave
 
What were your ratios of gold/HCl/HNO3? How clean has the gold been, did you remove basemetals first?

For the future (as Dave already said): Using urea is outdated. Just use as much HNO3 as absolutely needed, use a gold button to use up excess nitric or drive off NOx by using sulfamic acid...well, or deNOx by vaporising to syrup/adding HCl/vaporising to syrup/..., if you feel bored. All those processes are described on this forum.

There are some typical beginner's mistakes that can cause a failing precipitation:
excess oxidizer (here HNO3) and no clue how to remove properly or avoid it
failed to remove basemetals first (yellowish solution is a good sign)
too much liquid and too small amount gold in it (few and small particles are coagulating badly)
presence of large amounts of reducers like tin cations and/or organics (gold forms colloids or gets bound to complexes(?))
there is no gold in solution (failed to test / failed to dissolve completely / gold is cemented back in the solids / there is just no gold in the material)

Since urea forms critical products (try a search on the forum), I will leave it to the experienced people and the chemists here to advise how to solve your problem.
 
FrugalRefiner - Thank you for being as condescending as you were unhelpful. I thought this portion of the forum was to ask questions for people who need help. I didn't realize it is actually the place to go to have someone make gross generalizations about people and chastise them for not already knowing how to do everthing exactly properly. You may think I haven't read about as much as I can find about this process, however you would be incorrect. I have run across dozens of different "methods" for extracting gold - some of which I'm sure are just people guessing and consequently don't work. However, the method I used was the one I came across most often. If that is an antiquated process, that's fine - and that's why I came here to try to get help - because I don't know everything and am willing to admit it and as for help. If you are unknowledgable about the process or simply unwilling to help, that's fine, just tell me. However, if that is the case, I'm not sure why you're posting on the portion of this forum that is specifically for people asking questions because they are having issues...

solar_plasma - Thank you for actually trying to help me with this issue. As I stated to Frugal, I utilized the urea because it was the method I ran across most often in my research. Some people called for the use of zinc, magnesium, hydrogen sulfide, sulfur dioxide, ferrous sulfate, SMB, etc. I'm not sure what the best method is, but like I said, the one I came across most frequently was make a 3:1 ratio of HCl to HNO3 of AR, dissolve the gold with it, add urea to neutralize the HNO3 (which it does do, but if that is not necessary or an old method of doing so, I'm open to suggestions), then add the SMB to precipitate the gold. I added an additional step in there of first soaking the items in straight nitric acid to disolve out the copper and other trace metals and draining that fluid off to get rid of the majority of the trace metals. I'm not sure if that was a good idea or not, but I figured it wouldn't hurt to try as an experiment. Everything seemed to be going fine until I got to the SMB addition. I kept adding more and more SMB and it would fizzle and react. After I had added about 4 tablespoons (into about 100-200 ml of AR/gold solution) and it kept fizzling and never dropped out any gold, I figured I was probably doing something wrong. I searched and searched and could not find anything stating what I was doing wrong, but I didn't turn anything up in my research - hence the reason I came here to ask the experts. It made sense to me that the SMB was reacting with the HCl as the reaction between those components is:

Na2S2O5 + 2 HCl → 2 NaCl + H2O + 2 SO2

That is why I thought I may have to neutralize the HCl first - to keep the SMB from reacting with the HCl instead of precipitating the gold. Am I just missing something in my research/experimenting, or do I maybe just need to let the reacted SMB/AR solution sit longer to drop the gold out?

P.S. - I know this is not the smartest thing in the world to do, but I went ahead and added a SMALL amount of ammonia to the AR solution in order to lower the pH after I added the SMB which just reacted with the HCl. I know this could potentially create hazardous biproducts (silver azide, ammonium nitrate, etc.), but I just wanted to see if it would help with the gold precipitation. It actually worked great - gold fell out of the solution almost immediately. I would continue with this process if it were not dangerous. However, since it is, that is one of the reasons I wanted to come on here and see what I was doing wrong so I could proceed with my gold collection without creating hazardous materials...
 
Okay, you should stop right now and only ask, how you have to treat this mess, whithout being injured - and hope, someone will help you!

*period*

You obviously feel offended, but you don't have to. Dave is absolutely right and has given you the correct advice,, if you stay here long enough, you will find out, that he is a capacity on refining, just as there are a lot of capacities concentrated in this forum.

Take some facts as given, until you are able to verify them yourself: This forum is the one and only open source in the whole of the internet, that actually owns correct knowledge about refining, which is up to date. Forget what you have read anywhere on the net! Find the Guided Tour on the forum and read!
 
I am not the right person to tell you what to do now, BUT if you do the wrong thing right now, your acids will be capable of exploding right into your face without any visible reason. You do not have any clue, what you have produced.
 
Greetings cfoster78...

You may think FrugalRefiner maybe a tad harsh?... Just wait untill the rest of the "experts" have a say.
FrugalRefiner is just trying to instill the dangerous messes you are stepping into. Urea is fully covered here in the forum if you spend time reading here instead of "experimenting".
Even in Hoke's book it states to use as little nitric acid as you can. Does it mention anywhere about Urea neutralizeing HCL?
Everything I've read and learned, it doesn't neutralize HCL let alone a need to neutralize HCL in the first place.

I have noticed alot of people with chemical backgrounds having a tough time taking advice from anyone but even with your degree in Chemical Engineering,
you have much to learn about how to recover and refine PMs,(Precious Metals).
FrugalRefiner's response is more then justified and he is being kind in freely taking the time to answer your novice questions. Novice maybe not in the chemical background but n0vice in the field of recovery and refinning of PMs.

First and formost, what material are you trying to get anything from? And why are you even not attempting any of the "experiments" in Hoke's book?
It's the foundation for everything in this field.
After properly reading and understanding Hoke's teachings, read the welcome posts and it will guide you into the depths of this forum and help you answer your own questions.
Then, search the forum with the Google search on what material you have and how to process .

It appears you may have looked at her book but then went to the "Youtube will hurt you" videos and thought you're more then qualified to handle what you are trying to do. Nope...sorry but you need to understand the whole process from start to finish. Amonia added? Hmm...why? What does it actually do in AR?
The forum covers Amonia and it's importance. Covers what Urea does and why it's not used. As well as why you can't get any gold or anything to drop from your chemical mess.
Even I can see a problem when you stated your concerns with Silver azide, oxide maybe? Ammonia nitrate? Huh you be a goodt chemist. Read what you write as little spelling mistakes can be very costly to your health if you fail to take the time to be exact with any little details in this field.

Sorry you don't get spoon fed what you think you are entitled to. We all and that is "ALL" of us are entitled to Nothing. Nor are we obligated to do anything.
How's that for condescending?

Good luck and hopefully you will take this with a grain or 2 of sodium chloride and heed advise and learn the right way to be happy in learning PMs and how to see that nice pot ole gold at the end of the rainbow.

B.S.
...All the knowledge in the world is useless if one not follows those before...
 
cfoster78 said:
(snip)
P.S. - I know this is not the smartest thing in the world to do, but I went ahead and added a SMALL amount of ammonia to the AR solution in order to lower the pH after I added the SMB which just reacted with the HCl. I know this could potentially create hazardous biproducts (silver azide, ammonium nitrate, etc.), but I just wanted to see if it would help with the gold precipitation. It actually worked great - gold fell out of the solution almost immediately. I would continue with this process if it were not dangerous. However, since it is, that is one of the reasons I wanted to come on here and see what I was doing wrong so I could proceed with my gold collection without creating hazardous materials...
I sure hope you have your life insurance paid up in full as You could possible now have a bomb looking for a reason to go Boom.
NEVER add any chemicals together without knowing what CAN happen when you do.
Before you added the Ammonia to the mix you could have just added a copper bar and dropped all the PM's out of solution and started again.
Now I don't know how to solve your problem, so don't do anything without "Specific" instructions on how to fix this.

We NEED details of exactly what is in solution. ie. source of PM's and ALL chemicals along with all steps to get you to this point.
 
solar - I am not offended. It is actually very hard to insult me. I was just very confused about his response (and more so the manner in which he responded more so than the actual content). I have been researching this as much as I possibly can from a variety of sources. I have no idea which ones are good and which are bad. Consequently I have seen a variety of different methods - some of which I'm sure work, and some I'm sure don't. However, since I don't know enough about this particular process to know which ones will work and which don't, I figured I'd come on here in order to get help in determining the best method to utilize.

The only problem that I had with the response I got from Frugal was that it was obvious that he assumed I had not done my due diligence in trying to determine the correct answer myself prior to coming here for help. I am a scientist by profession as well as by mindset and I enjoy trying to figure problems out myself. I only ask after I have researched everything I possibly can and still can't seem to find an answer or get something to work. I'm not someone who looks for the easy way out and just asks people to tell me how to do things. I've been researching this process for better than a month, and have been experimenting by trial and error for about the past 3 weeks. While I do realize this is not an enormous amount of time, I have been trying to resolve this problem myself and have only decided to come ask for assistance because all I am doing is wasting money and materials by performing these trial and error techniques that are not working. I am safety conscious and have enough chemistry background with my degree in chemical engineering as well as real world experience to not do anything that is going to hurt myself or others.

I am basically just trying to get a little help on this topic as I have exhausted all of the resources I know of to get the answer on my own and I'd prefer not to waste any more materials trying to figure it out via trial and error. If this forum is not the appropriate place to ask questions, I apologize and would appreciate if you could directy me to a place that is appropriate for that purpose if you know of one. I was just hoping someone on here could let me know if I am making some sort of mistake in my processing based on the steps I listed out that I am taking in order to attempt to get it to work.
 
I make a simple comment about someone being condescending about me asking for help, and this is the response I get. Interesting...

I understand the dangers of the use of ammonia in this solution, which is why I stated I used a SMALL amount of ammonia in a small amount of the AR solution. I filtered the gold out, washed the gold thoroughly, and neutralized, diluted, and disposed of the remaining liquid in order to prevent a hazardous condition. Like I said, I know it can create dangerous biproducts which is why I limited the amount I produced and disposed of it immediately following the test. It is not something I am planning on doing long term, I was simply attempting to see if I were able to neutralize the acid with a material which did not contain any metal element if it would precipitate the gold given the SMB had already been added. It did, but since it can create dangerous biproducts I was not going to utilize that method on a large scale - hence the reason I came here for advise.

For those that are trying to help and asking questions about my process - thank you for taking the time to assist, and I will do my best to answer those questions. The gold I had precipitate came out a muddy orange color. I am utilizing electronic components (primarily from cell phones as I found a large quantity of old ones that were cheap). That (along with the SMB, AR and urea) is the only thing I have in my solution typically (except the times I tested other things, but I didn't plan on using them long term). I'm not looking to do this on a large scale or make money from it - doing chemistry experiments is just a hobby of mine and this seemed like an interesting one to undertake.

I understand the dangers of what I was mixing and new the potential biproducts. This is why I only made a small amount and disposed of it properly afterwards. I know enough about chemicals to know not to mix things when I don't have an idea of what the result may be. I thought about adding a copper bar (or zinc) in order to precipitate out the gold, but I figured it may have the same issue as the SMB had in that it would have to react with the HCl to neutralize the AR before it would precipitate anything out. I may be wrong about that, but since the SMB seemed to have that problem, I figured utilizing any metal replacement might as well.

To Pantherlikher - the urea idea was not from Hoke's book. That was simply a method I saw during my research from other books/websites that came up often. I know it does not neutralize HCl, it only neutralizes HNO3. That is why I came on there, to find out if I needed to neutralize the HCl prior to SMB addition since the SMB seemed to only react with the HCl if the HCl was not neutralized. Secondly, I know I have much to learn about PM recovery - that is why I am asking the questions and why I have been researching. I never claimed to know everything about it. If I did, I would not need to ask the questions. And yes, FrugalRefiner has every right to say whatever he'd like to say (just as anyone does). I was simply asking for help though, and did not see the need to answer in the way he did. If someone doesn't want to help, they obviously don't have too. I was just asking that he tell me that as opposed to jumping on me for not researching the topic (which I have done). I am also attempting several experiments. I only mentioned the ammonia one because that is the only one that has worked to this point. As for the going to Youtube comment, as I have stated, I knew what I was doing, which is why I took all of the precausions necessary to ensure safety (I have a fume hood with ballistic glass and only was using a very small amount of anything that would have created hazardous chemicals so if something went wrong it would not blow out my setup). As for the "problems" you saw - I actually did mean silver azide, not oxide. Silver azide can be obtained by crystallization from aqueous ammonia solution obtainable by double decomposition of silver nitrate and sodium azide in aqueous ammonia solution. And if you read my post, I actually said ammonium nitrate, not ammonia nitrate. So yes, I guess I "be a good chemist". Again, I'm not sure where the hostility is coming from. Although, if you are going to be hostile and make fun of me, it would probably be better if you were doing so about actual errors I have made. Neither of your examples fall into that category.

As I stated, I'm not looking to start a fight, not saying I know everything, etc. I simply am asking for help concerning a process that I have researched and attempted extensively but am having some problems with. I am more than happy to explain everything I have done, what materials I have used, etc. if someone is actually willing to help. I am not looking for people to berate me for asking a simple question. I'm sorry if I've offended anyone as that was not my intention. I was simply looking for help - and not looking for people to attempt to make personal attacks towards me for asking for said help.
 
So..yet again like others before you, you fail to see the problem.
It's not just an easy answer which you want. Can't happen. You have not even touched the surface of this forum as a resource so don't go there.

Read and learn what you are doing please before that Amonium nitrate makes another statistic.
Like everyone else, you justify your qualifications and defend your abilities instead of stepping back and looking at all of our answers to your inquest.

For starters, what did you start with and what steps you did to come to the conclusion that you are at a loss for what to do now? This will help us help you.

B.S.
...It is the humbled one who admits unknowing and begins to learn...
 
Nobody wants to offend you, they actually tried to help, but you are locked in your (wrong) beliefs and you are at this point not accessable to any help.

You know, I am a chemistry teacher. I had mastered to precipitate and melt some dirty pc gold and dissolve some silver platings (half of that silver I had vaporized, when I tried to melt it), before I came here. Further I am active in a hazmat team, even a medium leader. So, pretty much like you I came here and believed, that I was pretty well prepared and I believed I could find the last 10% of knowledge I was missing........*loooong breath*.......*rhethorical pause*........in a few days I found out, I was missing 90%..........after about a little year now, I know, I was missing 99%! Since I read every day since I came here, I still miss 80%. Edit: 80% only of what I am interested in and what I need for what I want to do in refining

So, calm down. Lean back. Do as they told you. And have a nice time reading.
 
Um... I nor anyone here tries to make personal attacks on anyone...against forum policy. As for silver azide, As I am no chemist, have never heard it exist. And have yet to find mention of it here in the forum. silver oxide yes.

You still have yet to let us help you. Step by step. You said some phone boards. great start. Did you depopulate? Did you remove solder? Did you use AP for other base metals? Nitric is a tad expensive and will..?.. make silver nitrate. Did you use that solution to add to HCL for the AR? You also mentioned reusing this AR from something else?

Being a chemist, why would you filter gold out of solution when gold is heavier and settles? Why would you not research this forum as you say you have exhausted every resource? Honest questions from a non chemist.

You keep saying you know enough to experiment yet you keep proving you have not read anything in the forum here. You do not need to experiment as it's already been done here in the forum with reproduceable results.

Lastly...most important question requiring an answer....
What exactly did you do with the solution to "dispose" of it?...

B.S.
 
cfoster78, your description, your conclusions and your methods .....I really don't know where to start.....begin at zero, believe me! :roll: You know...something... about chemistry and it will help you to learn easily from this forum, but read first for some weeks, before you even look at your chemicals again.
 
Thank you for the most recent responses. I did not realize you needed additional details in order to be able to determine what the issues are. I am more than happy to go through what I did step by step in order to give you a complete understanding of the process I used and hopefully be able to help me determine where I went wrong. And Panther - if you were not attacking, I'm sorry, I guess I just took it wrong. Calling out errors I typed (although they weren't actually errors) and saying "huh, you be a good chemist" seemed like you were trying to put me down. If not, I apologize for assuming that. As to your questions, silver azide is an compound that is explosive and unstable. It can be detonated by mechanical shock or an increase in temperature. Kind of like nitrogen triiodide, but stronger. As for disposal, I diluted the ammonium nitrate (as it is not harmful in solution - and is even used primarily as fertilizer), and converted the silver azide back to silver oxide, and with sodium hydroxide and glucose reduced the silver back to its metallic form and filtered it out of solution prior to disposal. The acids I of course neutralized prior to disposal as well. Also, I understand gold is heavy and will sink to the bottom of the solution, but getting that last bit at the bottom out is difficult for me to do just by decanting it, so I just pass it through a filter. It isn't too much of a hassle and it prevents me from accidentally pouring out any of the gold.

Now, for the process I initially tried using to get the gold, the steps I took were as follows:

I started with electronic circuit boards, pins, etc. from old cell phones. I cut out only the portions that contained gold so as to not have a lot of excess volume taken up by components that didn't have any gold on them. I did not however take off the solder, or anything else from the pieces I used. Consequently there would be some contamination of copper, lead, possibly silver, and any other components that would be on the boards along with the gold. Like I said, the only reason I cut out just the portions that contained the gold was so that I wasn't just throwing a bunch of metal and plastic in the solution that didn't have any gold on it. I did not however pick off any contaminants as I figured they would not precipitate out with the gold if I followed the correct process so it seemed it would be an unnecessary time consuming ordeal. I then placed all of the components into straight 70% nitric acid. I did this in order to disolve out the majority of the trace metals but not the gold (as gold only dissolves a VERY small amount in nitric acid). I discarded that liquid and then placed all of the components into HCl and began adding HNO3. I actually did try to use as little HNO3 as possible (as opposed to the standard 3:1 ratio for AR), but I'm sure that I probably put in a little more than was actually needed just to ensure I didn't put too little in and not be able to dissolve all of the gold. I let that sit and dissolve for 2 days. At that point I added the urea (although now I understand that step may be unnecessary) until it stopped reacting which told me the nitric acid had been neutralized. I then added the SMB. I only started with about 100-200 ml of the AR/gold solution, and after 4 tablespoons of SMB, it was still reacting violently (fizzing/bubbling) every time I put more SMB in, and no gold was dropping out. Since SMB reacts with HCl, I figured that maybe the HCl needed to be neutralized prior to the addition of the SMB. That's why I tried the neutralization of HCl with the small amount of ammonia just to see if it would assist in the gold precipitation, and it did. Again though, it is not a process I would do on a larger scale since adding ammonia can creat dangerous biproducts. It was simply an experiment to see if the neutralization of the HCl made a difference.

So my question would be, when you add SMB to the AR solution, does it normally take a lot of SMB to precipitate the gold out, and does it normally fizz and bubble a lot when you put it into the AR solution? If it does, maybe I just didn't add enough or didn't give it enough time to react completely. If it doesn't, I figure I may be doing something wrong. I have read you should only need to add an amount of SMB that is equivalent to the ammount of gold you precipitate. Based on my reaction, I would have needed to add a lot more SMB than the amount of gold recovered as all of the SMB was being used up reacting with the HCl.

And solar - I completely agree with you that I don't know much about PM recovery. That is why I came on here to ask questions about certain portions of the process so I can get a better understanding of it. I've been reading up about it, but I can't seem to find answers to specific questions that I have about the process that I was hoping I could get answers to here. While I know about chemistry in general - trust me - I fully understand that I don't know a lot about this particular process, which is why I was asking about it.

Thanks for your help.
 
Below is a picture of some cell phone board I have. They have been cleaned of most irony metals.
Is this what you put into your AR solution that you are asking about ???

I hope not, as they are Not ready for that yet. They still need to be depopulated to remove all the MLCC's and IC's which go to other processes to recover their values. Then they still need to go into an HCl soak to remove lead.

If you didn't do these steps first and just put everything into AR then you have NO gold in solution if you had a single piece of base metal that didn't fully dissolve.

We need to see step by step exactly what you have done so far. It would also be good to see pictures of what went into the AR and what came out of the AR.

edited spelling.
 

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I'm sorry niteliteone, I did forget to mention that. I did take off all of the electronic components such as processors, capacitors, resistors, etc. I just did not take off the excess solder and things like that. I did soak it in a nitric acid solution to remove unwanted metal, but not hydrochloric since pretty much all of the contaminant metals will dissolve in HNO3, but not all will dissolve in HCl (copper doesn't dissolve in HCl, lead does but very slowly, etc.) That's the reason I used a nitric acid solution to remove the unwanted metals as opposed hydrochloric acid. I unfortunately do not have any pictures of the solution however since it is the same solution I was experimenting with and have since disposed of it. I was waiting on making another solution until I figured out what I did wrong with the first one.
 
It's only fizzing, if you have excess nitric. If you have an excess, you process has been bad. You believe, you just need to ask a question, but the answer will only lead you to new questions. Questions, that you would easily have been able to answer yourself,if you would start reading. You could have searched for the right amount of smb per gramm of gold. You would have read, that an excess of smb could drive out some NOx maybe, but excess smb will precipitate copper as well (so, I can hardly believe your gold is something like orange, or this orange thing isn't gold), excess of smb will give a false positive stannous test and excess smb is waste of chemicals.

I love the high standards of this forum. If you don't want to learn to do things right, you will not get lucky here. Well yeah, you said this is why you ask. You can't ask all detailed BASICS without filling books with the answers! You will need to read them, as all of us have to.
 
Solar - I'm just asking one question. I'm not trying to get people to give me an detailed run down of the entire process. I neutralized the nitric acid with urea. I know you say that is an antiquated process of refining, but regardless, doing so means that I don't have excess nitric acid - and yet I still get the fizzing when I add the SMB. This seems to make sense since the reaction of SMB and HCl is:

Na2S2O5 + 2 HCl → 2 NaCl + H2O + 2 SO2

The SO2 is a gas and would account for the fizzing. Are you telling me though that when you add SMB to your AR, it doesn't fizz?
 

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