# Where did my gold go?



## 2002valkyrie (Oct 16, 2009)

Hi All,
I started with 17g. of 10k and 23.8g of 14k did my inquarting with 42.7g of sterling silver. This should equal 20.995g of refined gold and 67.005g of base metals. I used home made Nitric from Muriatic Acid and Nitric Soda to dissolve base metals then washed my black sponge. For the next process I dissolved the sponge in HCL and Bleach, filtered and then added Sodium Metabisulfite. (I did not dilute in H2O) I after sitting all night I separated it. I ended up with brown mud that totals to 7.8g. I checked the remaining HCL and Bleach with Stannous Chloride and it turns a little brown, I checked my Nitric solution which I also rinsed my sponge into and it turns dark black instantly. What should I do? I have considered using Aluminum to just start over. Anybody got a fix for me?


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## Anonymous (Oct 16, 2009)

Your first solution was a poor mans AR. if it were me I would put a piece of copper in there and let it cement out the gold and silver,
then start over, use real nitric for parting or try steves new cold nitric process seems it will yeild sulfate free or low sulfate nitric

Jim


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## Irons (Oct 16, 2009)

james122964 said:


> Your first solution was a poor mans AR. if it were me I would put a piece of copper in there and let it cement out the gold and silver,
> then start over, use real nitric for parting or try steves new cold nitric process seems it will yeild sulfate free or low sulfate nitric
> 
> Jim



Unless it's Chloride free, using Sodium or Potassium Nitrate to make Nitric Acid will dissolve some of the Gold. If the Nitric is dilute, the Chloride will precipitate out as Silver Chloride, contaminating the Gold.

You can check the Sodium Nitrate for Chloride by dissolving a little in distilled water and adding a few drops of Silver Nitrate solution.

The best solution is to buy some good quality Nitric.


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## eeTHr (Oct 16, 2009)

valkyrie;



2002valkyrie said:


> home made Nitric from Muriatic Acid and Nitric Soda


It should be _sulfuric_ acid and....

A quick way to make poor man's _aqua regia_ is to put, a little at a time, some dry sodium nitrate or potassium nitrate into the container of Au and Muriatic (31% HCl), until after awhile (especially if it's not heated) all the gold is dissolved (that way you don't have much nitric to get rid of before testing or precipitating). That's why the stannous test is black---it's _aqua regia_, not nitric.

(Plus what james and Irons said). There can be a little bit of chloride in the regular sulfuric-made nitric, too (something about the result of impurities in the sodium or potassium nitrate from the process by which they are made, I believe), so watch out for that as it can suck up a little of your Au if you don't get it out first.

Don


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## 2002valkyrie (Oct 16, 2009)

I used Hi Yield brand which Catfish had spoke about in the Forum Handbook 1st edition, pg. 21. As for cementing and starting over. What would be the best way?


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## Anonymous (Oct 16, 2009)

My suggestion was to put a piece of copper in to cement out the silver and gold,
then treat with nitric to remove the silver.
Jim


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## qst42know (Oct 16, 2009)

Or pure zinc turnings from Steve would be fast.


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## eeTHr (Oct 16, 2009)

valkyrie;

Also---


2002valkyrie said:


> I checked the remaining HCL and Bleach with Stannous Chloride and it turns a little brown



If you do this test on filter paper and get what looks like a coffee stain, it could be platinum, so don't throw that solution out. (Especially if it is orange as soon as you drop the stannous on it, then turns tan in a little while.)

Don


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## eeTHr (Oct 16, 2009)

valkyrie;

Here is one way I think you could recover your PMs from the two solutions you now have. I don't know if it's the best way, but it might be interesting to do. See if anyone else has any comments on it---

Treat both solutions as Au + Ag + copper + possible Platinum Group Metals.

With the aqua regia (first solution), get rid of any nitric with urea or preferably by the evaporation process (evaporation produces lots of toxic fumes).

Then dilute with 3 to 5 times water, this dilution with water will drop silver as the chloride form. Let the silver chloride settle and pour off or suck out the Au + Cu (+ PGMs?) solution into a new container, rinse the silver chloride with a little water and add this rinse water to the new solution container. A second rinse, or more may be optimal. There is always some fluid left in the precipitation, to avoid removing the precipitation with the solution. Avoid the use of filters whenever possible, so you don't have a bunch of filter papers to incinerate later.

Keep the silver chloride wet (add more water), save it until you have more or whenever you decide, then convert it to metalic silver using the lye and kayro syrup method.

Precipitate the Au in the new solution container with SMB, let it start to settle for awhile then test a drop of the solution for Au (if you get purple, add a little more SMB), let the precipitation settle for a couple of days, and pour/suck the remaining solution into a third container, rinse the same way again, into the third container. Your Au will remain in the second container.

Test the third solution for platinum and palladium with stannous and/or PGM testers if you have them. If it tests positive for any platinum or palladium, save up the solution, or whenever you want to, use the appropiate precipitation methods for those.

Do the same for the A/C solution, except just warm it for awhile to evaporate most of the chlorine if any is left over.

Don


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## 2002valkyrie (Oct 16, 2009)

eeTHr said:


> valkyrie;
> 
> Here is one way I think you could recover your PMs from the two solutions you now have. I don't know if it's the best way, but it might be interesting to do. See if anyone else has any comments on it---
> 
> ...



I'm a Noob but I would like to try if it's doable.

Here is an idea I have been tossing around in my head; If I can evaporate the Nitric off, what is stopping me from running it through a condenser and capturing pure Nitric? Or running the fumes through a pipit into chilled Hydrogen Peroxide for a Nitric solution? I know people make Nitric Acid that way but why can't I recycle? I got my eye on a condenser now.


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## eeTHr (Oct 16, 2009)

valkyrie;

I have seen that discussed on this forum in a couple of different threads. From what I have read, it is doable, but I don't remember the exact recommendations.

Also, I put some edits into my previous post. I hope they help. 8) 

Don

P.S. I am thinking about a condenser too, because it keeps the salts and chlorides out of the resultant nitric.


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## Oz (Oct 17, 2009)

I’m not going to go into all the advice that has been given so far but…

If I am not mistaken this is valkyries’s first precipitation. To keep things simple set aside any precipitate you have from SMB precipitation. 

Cement all the acidic solutions you have on copper until the solutions give you a negative stannic reaction giving you only precious metals as a precipitate from your solutions. 

Combine your 2 precipitations and process as a gold/silver/copper alloy with the possibility of PGM. 

You are then starting from the beginning then but with less base metals and the knowledge that your have gained.

I would save all solutions and solids from this first attempt to revisit later when your testing and procedure skills have been perfected some, just to be sure you did not throw out values. I would also use smaller amounts of PMs as you are learning this. 1 gram of gold content is more than enough to see in your beaker, wash, and make a bead from with a torch until you are more comfortable having success several times with smaller quantities before moving on to larger lots.

Keep it simple.


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## 2002valkyrie (Oct 17, 2009)

Thank you Oz, 
Simple, I think I will do that just to get some cash flow going. It is very sound advise.



Oz said:


> Cement all the acidic solutions you have on copper until the solutions give you a negative stannic reaction giving you only precious metals as a precipitate from your solutions.
> .



Forgive me but could somebody translate this phrase into a more Southern Alabama lingo for me please... Are you refering to the Stannous Chloride test? If so what should it look like? Anybody got a link to how to read the colors and reactions of Stannous Chloride? 

"Wow I read this and wish I had ask questions before I started... I hate learning the hard way."


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## Palladium (Oct 17, 2009)

2002valkyrie said:


> Forgive me but could somebody translate this phrase into a more Southern Alabama lingo for me please...




Translation = Roll Tide !!!


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## lazersteve (Oct 17, 2009)

Valk,

You should follow the Guided Tour Link in my signature line below. It will answer your stannous questions and many more. 

It always surprises me that so many noob's don't follow the links that have been set up just for them. Anyway, the guided tour will give you a list of reactions, reaction abbreviations and ingredients, safety tips, and much more. It's well worth the time spent reading in the knowledge you'll gain.

Steve


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## 2002valkyrie (Oct 17, 2009)

I have watched Lazersteve's video again (I have watched it many, many times because I am hearing impaired) I think I heard him say he droped the gold with SMB (Sulfate not Sulfite) I am really confused now because all I've read say's to use Sodium Metabisul*fite*. My drop looks nothing like his in the video. It took 12 hours to get a milky brownish tan mud and his was a noticable black in a matter of seconds.My acid stayed yellow and his cleared instantly... :?: Thoughts anyone? :?:

This is a link to his video.http://www.goldrecovery.us/goldrecovery/videos/smb.asp


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## lazersteve (Oct 17, 2009)

The video audio was a slip of the tongue. I haven't had time to remaster the audio portion to repair the discrepancy. It's *Sodium Meta Bisulfite*.

The reaction will vary depending on concentration of gold in the solution, temperature, free oxidizers (e.g. chlorine, hydroxide, NOx). If you only have a small amount of gold in a large volume of liquid you will get the symptoms you describe. 

The persistent yellow tint is likely either chlorine (more green tint), iron ( more yellow orange), or gold with too much oxidizer. The excess oxidizer redissolves the fine gold as soon as it is precipitated.

This is where stannous chloride tests are used to let you 'see' if the gold is in solution before and after adding SMB.

Steve


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## 2002valkyrie (Oct 17, 2009)

Thanks again Steve, you are the goto guy no doubt.


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## Oz (Oct 17, 2009)

Sorry about that. Yes, I was referring to a stannic chloride test reaction. 

As to colors if there are multiple PMs present it can become hard to read without experience. You will notice in Hoke that she recommends acquaintance tests with known pure metals, and if I remember properly even suggests you mix some PMs in different ratios to see the difference. 

For your purposes here on your first process any color change you will see on a stannic test indicates you still have values in your solution. For reference, gold by itself can give reactions from light purple (low gold content) to black (high gold content). 

Something that is exceedingly important is that you are sure your stannous chloride is functioning properly or you risk throwing out values that you do not see because of bad stannic. A very easy way to be sure of your stannous chloride is to make a gold test solution. 

Find a discarded computer card with a gold finger edge, trim the edge off and use AP (HCl with just the smallest dash of H2O2 (hydrogen peroxide) to remove the copper from under the gold platting) until you have the gold foils floating free. Filter out the gold foils and rinse. Put your foils in a test tube and add a small amount of HCl and add unscented household bleach a few drops at a time until your gold dissolves (gentle heat helps). Keep this auric chloride (known gold solution) on hand.

Now every time you wish to test for values in solution with stannous chloride you can first test to see that your stannous is reacting properly by using your “known gold solution” before you trust it to test something more valuable.

As you test with stannous the colors will become more familiar. PGMs get a bit more involved but not terribly. This is also why I suggested you save solids and liquids incase you do have some PGMs in your karat gold.


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## eeTHr (Oct 17, 2009)

valkyrie;

Here are some in-depth Questions & Answers about stannous chloride use, plus some interesting stuff about precipitating.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=41&t=5271


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## Oz (Oct 17, 2009)

2002valkyrie said:


> It took 12 hours to get a milky brownish tan mud and his was a noticable black in a matter of seconds.My acid stayed yellow and his cleared instantly... :?: Thoughts anyone? :?:



Your brownish tan is dirty gold, your milky white is silver in solution reacting with chlorides to form silver chloride.


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## 2002valkyrie (Oct 17, 2009)

What should I do with it? :?: Dump it in with the rest of the mess?


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## Oz (Oct 17, 2009)

This will get very convoluted receiving advice from multiple people at this point given what you have already done. I would suggest that you pick one person to guide you through this in private messages without distractions as too many cooks spoil the brew. The problem is that there is more than one way to solve this but trying more than one method at a time will not work. 

I believe in the KISS system, keep it simple stupid.

As for you question on what to do with your current precipitate, the silver chloride you have made will not be affected by nitric, HCl, or AR, but will ride through the process and be saved so you can convert it to silver metal once again later. For now your focus should be on the gold you have invested in this process in my humble opinion. This is another reason I asked you not to throw out solutions or solids from this even if you “thought” they were worthless.


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## eeTHr (Oct 17, 2009)

valkyrie;

After thinking more about your solutions situation, I would have to say that I think the copper cementing method has got to be the best place to start. The reason is that it will leave the copper (from the sterling) in solution, and thus keep it out of your way for the remaining steps. This follows the "eliminate the base metals first" rule, which makes everything else much easier and more efficient.

And doing it all in one big batch would take fewer steps. Your existing precipitate will go through the process OK.

When you decant the solution into another container (rinsing as mentioned before) after letting the copper metal work a few days (copper takes awhile), you will have only PMs precipitates (including the silver chloride riding along) left in that container.

Transfer the copper metal to the new solution container to see if any more comes down. It can still produce a little powder up to about a week later. When you're done with this solution, put some nails in it to drop the copper out. To further neutralize the solution for safe disposal, see 4metals' post at http://goldrefiningforum.com/phpBB3...40831&hilit=safe+disposal+of+chemicals#p40831

Then dissolve your precipitates in your manner of choice, evaporate accordingly, dilute, decant your PMs-bearing solution from the silver chloride (store the silver chloride covered with water), drop the Au out of the solution with SMB, and save the rest of the solution if it tests good for any PGMs.

Suggestions by others are always welcome.

Don


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## 2002valkyrie (Oct 17, 2009)

How do I know when I have evaporated the Nitric Acid off? Is there a good method? I figured Harold would have posted a method but I have not found it as of yet.


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## eeTHr (Oct 17, 2009)

When you evaporate it down to the point that it starts to get syrupy, add a little HCl. If there is still nitric in it, that will make the nitric fume. If there is still nitric in it, add more HCl and evaporate it down until it starts to get syrupy again, and test it again with a little HCl.

If you only add a little nitric at a time until all the metals are dissolved, especially with a little heat, it usually only takes one evaporation. Some people don't evaporate at all when they do it this way, because all the nitric is consumed by the PMs.

Also, if you add a little sulfuric acid, about 1% of the volume of your solution only, it will drop any lead chloride (which you probably don't have in this batch, as it came from karat Au) and it will help to get rid of the nitric. You only add it once, at the beginning, because in won't evaporate except at much higher temperatures.

I evaporate mine at 190 degrees surface temperature, and turn it down to 140 or 150 toward the end, because once it gets down to a certain level it will spatter when it passes through a certain ratio of nitric to HCl.

Edits for errors: Adding the sulfuric drops the lead as lead sulphate, not chloride.

The spatter is due to the ratio of nitric, HCl and/or water. Apparently, at a certain ratio of these, the boiling point of the combination drops suddenly, and instant boiling causes the spattering. See link---
http://en.wikipedia.org/wiki/Aziotrope


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## Harold_V (Oct 17, 2009)

2002valkyrie said:


> How do I know when I have evaporated the Nitric Acid off? Is there a good method? I figured Harold would have posted a method but I have not found it as of yet.


Harold isn't willing to get involved in a fray such as this. Resolution for the problem is simple, but as long as opinions are posted freely, all my suggestions would do is continue to muddy the water. 

Oz gave you excellent advice. That is to resolve this issue privately. While there are several routes that can be pursued, following the advice of one person, staying the course exactly as advised, is the wisest thing you can do. All too many readers have less than enough experience to understand the ramifications of some of the suggested procedures. There is an optimum method that can bail you out.

When you tested your supposedly nitrate solution and got a black reaction, that should have sent up a red flag for you. You have dissolved values in the first digest. That is where your missing gold will be found. Do NOT discard anything at this point in time. You can achieve what is, for all practical purposes, a 100% recovery, as long as you still have all of the material that has evolved from your various processes. 

Harold


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## eeTHr (Oct 17, 2009)

Harold;

While I took a cautious stab at it, I would certainly value your opinion over my own.

I think most people on the board would like to see how it should optimally be done.

Could you pleeeeeease give (most of) us a learning experience?

Sincerely,

Don


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## qst42know (Oct 17, 2009)

> Harold isn't willing to get involved in a fray such as this. Resolution for the problem is simple, but as long as opinions are posted freely, all my suggestions would do is continue to muddy the water.



I fold. Please lead on.


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## 2002valkyrie (Oct 17, 2009)

Once again, I seem to have embarrassed myself through this forum... 
I halted all my procedures and realized I had problems when my 1st batch dropped too slow, too little and off colored. Then proceeded to start investigating with measurements including a stainus test in order to give the most information to the forum and try to turn a bad experience into a learning one, so that I might learn from my first blunder. As of from the time that I put the brakes on my processes I have only asked questions, gathered information and tried to process through it with as much common sense as possible. I have froze all my activity and will wait until I have found some confidence as I lost all of what little I had. 
(*Please understand the title of this thread was to get the attention of wiser minds than mine, I know the gold is still in a vessel in my work area and is recoverable)* The questions are: 
1) What can be learned from my ignorance? 
2) What is the best way to come away with gold and silver without adding to my waste any more than is necessary?



Oz said:


> This will get very convoluted receiving advice from multiple people at this point given what you have already done. I would suggest that you pick one person to guide you through this in private messages without distractions as too many cooks spoil the brew. The problem is that there is more than one way to solve this but trying more than one method at a time will not work



I would like to say; "As part of my quest to gain some confidence I have sent private emails from the beginning to a few intellectuals asking various questions and opinions."This public forum is just one way to get more attention to my embarrassment and answers to questions that are not answered in private as well as share my mishap so maybe others might benefit.



Harold_V said:


> Harold isn't willing to get involved in a fray such as this.



I have only the upmost respect for Harold and only mentioned him as I know he has mentioned "evaporation of Nitric was his preferred method" but I have not read any specific procedures of his on the forum . And as much as I value his input, I also understand and respect his not wanting to be involved in this "fray" of mine. He is right to call it such. I have messed up and even though it's my embarrassment and frustrations that teach me the most, it is the harsh words of wiser men that cement my learning experience. And if he were to make suggestions as to what should be done. I would certainly take notes along with the educational criticism he sends my way. I know from reading the forum that there is no candy coating that goes with him, I respect that the most. 
"I hope this offends no one and we can continue this thread with the best intrest of all Noobs in mind as I am the noobest Noob and value all of the brain power on this forum."


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## Oz (Oct 18, 2009)

I doubt that you offended anyone, certainly not me. I understand that you were just trying to get all the information you could. My suggestion was because I was reasonably sure that this was your first precipitation attempt and the multiple processes being suggested differed significantly enough to cause you confusion instead of help.

It is good that you wish this to benefit others. Perhaps after you have worked through this with one of those you have been PMing with, you could report back the steps you took to resolve it.


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## Palladium (Oct 18, 2009)

2002valkyrie said:


> How do I know when I have evaporated the Nitric Acid off? Is there a good method? I figured Harold would have posted a method but I have not found it as of yet.



I'm glad i don't answer questions, I just post links for reading.  

Harold has stated several times that he always added a button or small piece of gold so the excess nitric would be use up. 

Here's a good conservation in the middle of another topic. :arrow: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=4674&hilit=evaporating+nitric+excess&start=20

And here's a different type process, but same principle.

http://goldrefiningforum.com/phpBB3/download/file.php?id=2899

Dissolving the Filings and Gold Mud With Aqua Regia

Place the filings in the same beaker as the brown gold mud, and add one (1) ounce nitric acid and four (4) ounces HCL for
each ounce of gold that you estimate is to be recovered. Filings will actually use more acid than the brown mud as they still
contain traces of base metals. Add the acid slowly to avoid the beaker boiling over. The idea is to add a small amount of the
acid mixture (aqua regia) and let it work, then add more. If all is added at once, the filings and fine gold powder go into
solution immediately, with a sure boil over. The beaker should be placed on the burner and allowed to boil at a low heat until
all the acid is used up or all the metal is dissolved. Don't use any more nitric acid than you need, as it must all be used up
before the gold can be recovered by precipitation. An excess of HCL does no harm, and insures all the nitric that is able to be
used up is used up as it reacts with the gold.

Evaporating the Gold Solution

Once all the acid is used up, or the gold is totally dissolved, take off the watch glass, pour in a little HCL to cool the solution,
then pour in a few drops of sulfuric acid. Be sure to stir with the glass rod all the time the sulfuric acid is being dribbled into
the beaker as it will want to flash to steam. Sulfuric acid is the method one uses to expel lead in solution. It converts it to
lead sulphate, which will be filtered off when the solution is filtered after evaporation. Lower the heat and allow the solution
to slowly evaporate. Do not evaporate too fast. Gold will be lost. After the solution gets concentrated, weigh a gold button
and record its weight on your tracking sheet. Slowly introduce the gold button to the beaker (DON'T DROP IT IN) using
tweezers. One should add some HCL at this point. The beaker should still be on the burner. If the button doesn't begin
bubbling shortly after it is introduced, all the nitric acid has probably been used up or expelled by evaporation. That is
unlikely. If no bubbling is noticed, evaporate the solution until it starts to thicken and leans towards a red color, then remove
it from the burner and add about four (4) times its volume of water to it to cool it. Stir it as the water is added as the gold
chloride will readily cool to a hard lump if it isn't diluted. You will need space in the beaker for wash water from washing
down the funnel and ice when you precipitate the gold, so don't use excessive water at his point.

You will more likely find that the button bubbles, as it is being dissolved, using up the free nitric acid. Keep it on the low
heat and add more HCL when the solution thickens and darkens. You will notice that each time HCL is introduced the button
starts the bubbling all over again. When HCL is added and it doesn't bubble, there is no longer any free nitric acid. Treat the
solution from this point just as above, removing it when it thickens and leans towards red in color. A cautionary note. When
the solution has gone too far in evaporation, gold will precipitate. As water is added, the solution will look something
like brass paint, in that small particles of gold will be noticed, suspended in the solution. Should that happen to the lot, put it
back on the burner and drop in a little nitric and HCL. Try to use a one (1) to four (4) ratio, as you are now building a small
amount of aqua regia to re-dissolve the gold that has precipitated. Repeat the evaporation as above, using excessive HCL to
insure total expulsion of nitric. One must evaporate the solution until it thickens somewhat, otherwise the free HCL makes it
difficult to filter. The filter paper wants to break through when the acid level is too high. About all that can be done when
that happens to you is to either dilute the solution with water or get it back on the burner and evaporate it all over again.

Harold


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## 2002valkyrie (Oct 18, 2009)

Palladium said:


> I'm glad i don't answer questions, I just post links for reading.



This sounds like good sound directions to follow once I get out of this pickle I'm in and start over. Thanks alot for the links, I like step by step proceedures and wish I had read this before, I would have noticed my problems a little earlier.


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## Harold_V (Oct 18, 2009)

I didn't mean to come across as an old crotchety dude (although I am one) with my comments. The problems I mentioned are all too real, especially when coupled with an individual that deems it appropriate to tell those of whom he is asking advice only that which he cares to disclose. I've been through that on more than one occasion. I have no intentions of doing so again. 

Clearly, that is not the case here, and I am not making any accusations. 

GSP and I have, combined, probably 70 years of refining experience. He and I do not agree on many subjects----although I hesitate to say that either of us is wrong. I have my reasons for the position I hold, and I'm sure he has his as well. Both of us have refined more gold that most folks can hope to see in a life-time, each with acceptable quality. 

The problems start when one asks advice and two (or more) methods are recommended, then the individual making the inquiry decides to pick from each, that which appeals to him/her for what ever reason. When things go south, it borders on the impossible to understand why, especially when the method suggested has worked flawlessly previously. 

Yes, there are various processes one can pursue in recovering from an incident such as this. My procedure may be better, or worse, depending on many variables. 

Here's what I'd do if this mess was mine. Lets start by determining that the material, inadvertently, was processed with AR, regardless of the best of intentions. That means that everything in the alloy except silver has been dissolved. The silver would have been converted to silver chloride, which should be expected. 

My logic in this case is simple. I'd recover all of the dissolved values without attempting to recover any of the base metals. Therefore, zinc is out. As has been suggested by more than one individual, I would recover the dissolved values on copper. I would use pieces of copper that present a large surface area to the solution, and I would leave the copper in the solution until the solution checks barren with stannous chloride. I would then remove the copper and wash each piece carefully, recovering all traces of the black cemented particles, which are the values. 

To address the silver chloride, I would have washed it well with water (tap water is fine--it is already a chloride---what possible benefit one would gain by using distilled water?), combining the wash water with the solution that was cemented with copper, above. The remaining solids I would then reduce to elemental silver, using scrap iron or aluminum. It's important that the conversion be accomplished with metal, so traces of values, which are sure to remain in the silver chloride, will be recovered as well. 

When the cemented values have been well washed, I would incinerate them, to insure that there are no chlorides present. I would then process in nitric, to eliminate any traces of base metals that have hitched a ride. The results should be relatively pure gold. 

I would incinerate the silver, which would have been recovered with metal, then I would process it with nitric, which would yield the traces of values that likely got included with the silver chloride. I would recover the resulting silver nitrate with copper. I would add the traces of vales to the gold from the previous digest, at which time I would dissolve the solids, evaporate, filter, then precipitate. 

In this particular instance, while evaporation has been discussed as a method of eliminating nitric from the original digestion, that is not a good idea, nor is it required. Evaporating solutions that are heavily contaminated with base metals can be troublesome, especially when a serious amount of silver chloride is included. When it has been determined that a process has gone awry, it is usually far better to get back to square one and start over than to attempt to live with the problems. A total recovery would be using scrap iron or zinc, cementing down all values, along with copper. In this case, it's clear that recovering the copper will serve no useful purpose-----therefore using copper (for cementation) is the wisest choice. 

2002valkyrie , you asked about starting over, using aluminum. Unless you have more experience in refining, I suggest you avoid using aluminum. It presents more than a lion's share of problems once introduced to your solutions. They can be handled, but it may not be apparent how, or why. If you find yourself in trouble and must start over, consider copper first, then iron (steel, not cast iron) or zinc. 

Harold


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## eeTHr (Oct 18, 2009)

Harold;

Whew, thanks very much for posting. Your wisdom, time, and effort is a great help, and much appreciated!



Harold_V said:


> The remaining solids I would then reduce to elemental silver, using scrap iron or aluminum.


What type of solution should the silver chloride be in to do this?

I'm getting that in this particular case, with mainly just silver chloride present, the use of aluminum would not present the problems which you mentioned in your last paragraph, as one would be "done" with the solution afterwards anyway?

Don


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## goldsilverpro (Oct 18, 2009)

Good post, Harold. Pretty much the way I would do it, also.


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## 2002valkyrie (Oct 18, 2009)

To everyone reading this post,
I have researched all my options and though many of you have offered good advise, I have decided to take some and handle this blunder through the private messaging route in hopes that I will not only resolve my problems but also learn a little more in depth as well as hopefully gain a friend. I will hold back my posting until I can post in full my route to recovering my pm and also refined it as I intended to. As for the intellectual that is helping me, they must authorize me to disclose their identity. 
Until I post again, Thank you all for your concern and advise.


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## 2002valkyrie (Oct 18, 2009)

2002valkyrie said:


> I have decided to take some and handle this blunder through the private messaging route in hopes that I will not only resolve my problems but also learn a little more in depth as well as hopefully gain a friend



Well maybe not I have tried to use the P.M. feature so many times. I'm tired of typing the same thing over and over. There is an issue with the P.M. feature.


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## Harold_V (Oct 19, 2009)

Harold_V said:


> The remaining solids I would then reduce to elemental silver, using scrap iron or aluminum.





eeTHr said:


> What type of solution should the silver chloride be in to do this?


All of my experiences with silver chloride were handled with a water and HCl solution, the sole exception being the silver chloride that was recovered in the furnace. 

In the case in question, I would have rinsed (with tap water) the silver chloride a couple time, to remove the majority of contained values, then I would put the material in a vessel that can withstand heat (from the reaction), covering the material with water, then adding about 10% more in HCl. I would then introduce scrap aluminum (or scrap steel). I used aluminum because I had an abundance, and was willing to deal with the problems (inability to filter until well rinsed).


eeTHr said:


> I'm getting that in this particular case, with mainly just silver chloride present, the use of aluminum would not present the problems which you mentioned in your last paragraph, as one would be "done" with the solution afterwards anyway?


The problems are real, and they persist when reducing silver chloride. The one advantage is that you can rinse the resulting material endlessly, allowing the solids to settle well, then decant by siphoning. That leads to considerable confusion, because the solution now appears much the same as the resulting silver, so you have the never ending question of losing silver, or not. My experience indicated to my satisfaction that none was lost, that it was the aluminum that created the appearance. 

Once well rinsed, the resulting converted silver will filter perfectly well, but it's very important that you rinse several times before attempting to filter. 

If you have any doubts, use scrap steel. Nails cost too much, and they aren't really the best choice because in the end it's required that you remove any unused metal. Starting with sheet material, presenting a large surface area, is best. If one scraps computers, many of the covers are made of steel that is not painted. It's perfect for the job. Any traces can be dissolved with HCl after the converson has taken place. That is one of the reasons I chose to use HCl in lieu of H2SO4. There is no risk of dissolving any of the converted silver. 

Be cautious of using pieces of scrap steel that are quite thick and heavy, for you will be inclined to break the vessel in which you are making the conversion. The silver chloride should be stirred on a regular basis, so all of it comes in contact with the scrap material being used to make the conversion. 

Harold


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## eeTHr (Oct 19, 2009)

Harold;

Thanks for the very detailed explanation. There are so many things that can happen when trying a new process, that it really helps to know ahead of time what to expect, and what to avoid. 8) 

Don


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## 2002valkyrie (Oct 30, 2009)

2002valkyrie said:


> To everyone reading this post,
> I have researched all my options and though many of you have offered good advise, I have decided to take some and handle this blunder through the private messaging route in hopes that I will not only resolve my problems but also learn a little more in depth as well as hopefully gain a friend. I will hold back my posting until I can post in full my route to recovering my pm and also refined it as I intended to. As for the intellectual that is helping me, they must authorize me to disclose their identity.
> Until I post again, Thank you all for your concern and advise.




Well it has happened... I found my gold. :lol: 

It took a little while as I went ahead and spent the bucks and purchased Nitric Acid $114.00 / 2.5 liters. I will save the work around methods till after I have refined myself to a second nature.
I have permission to tell everyone here that it was Harold V. that held my hand and tutored me, we used Hoke as the handbook (Bible) for this study. I know it took 12 full days but all my gold was recovered and I have learned so much my head hurts. I am ready to start my second batch and this one will be by the book (HOKE). As everyone here already knows Harold is a very good teacher and though he tells it like it is, he is a friendly one also. SO if he says something you don't like or rubs you wrong, step back think it through, you will more than likely see he has a good reason for what he says.  

_*Thank You Again Harold V*_. I hope it wasn't too bad an experience. 
* Thanks to everybody for making this forum the greatest!*


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## Harold_V (Oct 31, 2009)

My pleasure, 2002valkyrie, although you reaffirmed my hunch that it's very difficult for those that are learning to not get creative and make decisions that are counter-productive. No matter, you landed on your feet. My hat's off to you!

I have a very straight forward approach to gold refining. I use a method that is known to work, and work well. It may or may not be the fastest or easiest, but it is a sure thing. 

I learned it all from *Hoke.* 

Harold


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## Oz (Oct 31, 2009)

This is to the both of you, Valkyrie you chose a fine tutor.

I have never met a machinist that was not “old school”, it is a dying trade with computerization, but it requires a meticulous mindset when you are not just punching a keyboard. 

Old school teaching can seem abrasive to many of the newer generation, it is their loss not understanding the value of this method of teaching. 

This old school mentality still persisted in Germany when I lived there and it required 6 months of school to be allowed to flip burgers at McDonalds. While I did not feel the need for such with a burger, tell me of a product out of Germany that is not considered quality (this may mean more to machinists).

The value of a trade, the apprentice, and the respect required of elders with vast knowledge has been lost on the masses. 

It is a joy to hear you understood this and took the high road.


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## 2002valkyrie (Nov 10, 2009)

Here is a picture of the elusive gold that I learned the hard way with. This should give this thread the proper closure. I will be selling the button it weighs 32.4 grams = 20.8 dwt = 1.04 ounces.


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## eeTHr (Nov 10, 2009)

Nice color.

It looks like some nice crystalization on the button, and the shot looks like Harold's famous "Bowl o' Gold."

8)


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## Oz (Nov 11, 2009)

Very nice indeed! 

Seeing the color leads me to believe you cooled the button slowly playing the torch a bit since you have grain on the edges but no piping. 

Way to go!


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## 2002valkyrie (Nov 11, 2009)

Thanks for the complements ya'll (Alabama) but as I said in my postings. I had help from a very seasoned veteran who I owe more than a simple thank you. It is my wish to show Harold my appreciation through much success and hopefully one day be able to pass along the favor in his name as he did in Hoke's. His name is certainly well known in my house... 

On a positive note. :arrow: 

I have been able to replicate my success with 2 other buttons. 8) Man I need a buyer... So I can do it some more! :lol: 
:!: Addicted, I am :!:


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## LeftyTheBandit (Nov 11, 2009)

Well done Valkyrie!

Your success is a testimonial to how this board and the Harold can have a positive out-come to a bad experience if listened too. 

I'm sure Harold feels a new pride knowing that there are new-comers that are willing to listen to tried and true methods and follow these methods to the letter. By looking at your button, I'm sure Harold feels a certain accomplishment from your success. I hear he likes Canadian Rye Whiskey "Crown Royal".


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## 2002valkyrie (Nov 18, 2009)

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=6015


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