New and lost!

shop deals on amazon
xelexo
Advertise with us
Shop deals on ebay
Gold Refining Forum

Help Support Gold Refining Forum:

This site may earn a commission from merchant affiliate links, including eBay, Amazon, and others.
H

howdee500

Member
Joined
Jan 22, 2013
Messages
9
I am reading and rereading Hoke,unfortunately not before using an "easy" receipe found elsewhere.
I started with about 95 grams of various karat scrap jewelery to include an old rolled gold watch case and possibly a lapel pin or 2 that may or may not even contain gold also there was 1 white gold earring. For some DA reason, I started right out with AR. Yellow cloud etc.(bye-bye gold?) reaction stops, heat in boiling water. Dark green almost black liquid with only partial disolve, let set overnight no change. Noticed one small piece of 18k had a grey coating, silver cloride? I strained the hole lot and went with nitrate and water 50/50 which also turned dark green not blue then back to more AR. This also dark green liquid has been heating without disolving anything for about 2 hours and these are delicate pieces. I can even see tiny gold computer pins ( the flat kind) floating without even discoloration. The only things completely disolved are light chains and that rolled gold watch case. My AR is very dark with black scum.
Having saved all solutions, I have urea and smb and have not deluted either AR.
I have deluted the nitrate 50/50 and added salt mixture.
Would very much appreciate any help
 
You are dealing with Karat jewelry, you are going to need to inquart. You need to search for how to inquart.

This is why your jewelry is not dissolve in AR or Nitric 5'0/50. The silver is preventing the gold from dissolving in AR, and the gold is preventing the silver from dissolving in Nitric.

When you inquart, what you are actually doing is increasing the silver or "upgrading" the silver content so you can dissolve it in nitric acid, leaving behind the gold.

Hope this helps

Scott
 
Hey Scott,
Thanks for the quick reply, Yes I found about inquarting to late for this batch. However, didn;t Hoke refer to using a variety of Karat pieces as an alternitive of sorts. A 9k gold rolled watch containing lots of copper, a bulk of 10-14k with a single tiny 18k bell.
It is now desolving slowly, all but one ring and those tiny computer flakes???
So having lost my shot doing this batch correctly by inquartation is there any hope for me to precipitate my gold from this motor oil looking AR?
Thanks
 
Yes, if there is any gold in the AR solution you can expand your solution, with water, and then test with Stainnous Chloride for a positive color. If it tests positive for gold, then you can follow the correct procedures for precipitating your gold out of solution from that point forward.

If your solution is too thick, you are going to have a really difficult time precipitating any gold out of your solution.

If you have excess nitric acid in solution, you are going to create NOx as you add SMB. I would try burning off the nitric instead of using Urea. When you are dissolving metals in AR, it's best to make small additions of nitric acid until all your metals are dissolved, rather than making a by the book 3/1 solution of HCl/HNO3. In this way you are not using excess amounts of nitric acid, so don't have to deal with it after everything is dissolved.

When you inquart, you have to melt the metals together into a homogenous melt before you attempt to dissolve it in Nitric Acid. There should be clear instructions on how to inquart on this forum, I believe there are even videos somewhere. But it's important to get a nice homogenous melt before you pour it out so that the Nitric Acid will attack the silver and only leave behind gold.

Scott
 
Scott,
By burn off you mean heat (not boil) and evaporation? After which I dilute with water or hydrocloric if to thick? What about the dark green. Lots of copper and probably silver. With these precipitate along with the gold? If so, would you recommend treating the dry mud with a bit of nitric 50/50 and then AR again or will the washes surfice?
Thanks again
 
howdee500 said:
Scott,
By burn off you mean heat (not boil) and evaporation? After which I dilute with water or hydrocloric if to thick? What about the dark green. Lots of copper and probably silver. With these precipitate along with the gold? If so, would you recommend treating the dry mud with a bit of nitric 50/50 and then AR again or will the washes surfice?
Thanks again
Click to expand...

By burn off I do mean heat, not boil, good point, add small amounts of HCl when you burn off the Nitric, then after when you filter, do so into water with ice in it, the precipitate. Your first refining is going to be dirty. So after you precipitate, decant, wash several times and you know there is no more acid, incinerate, then digest in Nitric Acid to dissolve most of the base metals, decant, wash, digest in AR again, precipitate, and move forward from that point on.

Scott
 
When you used aqua regia on the various types of scrap you attacked some of the gold, but the acids will attack the base metals easier, and the gold will cement back out of solution if there is enough base metals to cement it out. This puts some of your gold into finely divided powder more easily lost.

Gold fill can be most any metal, even some of the very troublesome metals, that you really do not want in a solution with dissolved gold, I would not mix gold fill or plated gold with karat gold, too much of a chance to lose gold, or make things much more difficult.

With out lowering the karat of your gold the silver will become a problem for aqua regia, and gold is a problem for nitric acid.

You had a lot of base metals in solution, your strong acid was attacking them, what gold was attacked could be plated back onto and copper or other base metal that did not dissolve, like the computer pins you saw floating and not being attacked.

Also the gold fill could introduce tin into solution locking up some of your gold as those dreaded gold robbing colloids.

When you used aqua regia on the karat scrap some gold dissolved, but the silver in the metal made a protective crust of silver as the gold dissolved away from the silver, this silver chloride crust would not let aqua regia attack any more gold silver or other metal from the karat gold.
When you moved these to nitric acid it would not dissolve the silver crust as silver chloride will not dissolve in nitric acid, but you have now introduce chlorides to that nitric acid which will now dissolve gold (you just made Aqua regia out of that nitric, although it is made up of mostly nitric acid and very little HCl), also this solution will be a bit harder to test for gold as most of the solution is nitric acid or nitrates, one way I may try to get my gold back from that solution is (save it, and reuse it later), dissolving silver it will form silver chloride which will precipitate as white powder(removing any chlorides or HCl that is involved).

Basically I think you need to spend more time understanding what Hokes is trying to teach you, following what she teaches, that way you will not end up with all of these troubles, and would not be loosing your valuable gold from all of the different ways you could have been losing gold such as the way you did this batch.
 
Hey Scott,
I'm cooking the AR down using a crock pot with 2" of water. The AR is in a pyrex cake mix bowl over a saucer to keep it from direct contact with the element. I am trying to keep the water just under boiling but often unsucessfull. Th AR however is not quite to a boil.
The thing is, a green crust is now forming over the entire solution and on the sides of the pyrex. This crust is easily broken and desolves, but reforms in a couple of minutes. Just wondering what it might be.
I am down about 1/2" of evaporation in a vessel 6" dia. and AR now only 1" deep, all metal solids gone. Time to add hydrocloric? water?
Howard
 
howdee500 said:
Hey Scott,
I'm cooking the AR down using a crock pot with 2" of water. The AR is in a pyrex cake mix bowl over a saucer to keep it from direct contact with the element. I am trying to keep the water just under boiling but often unsucessfull. Th AR however is not quite to a boil.
The thing is, a green crust is now forming over the entire solution and on the sides of the pyrex. This crust is easily broken and desolves, but reforms in a couple of minutes. Just wondering what it might be.
I am down about 1/2" of evaporation in a vessel 6" dia. and AR now only 1" deep, all metal solids gone. Time to add hydrocloric? water?
Howard
Click to expand...

When the metals start to crystalize like that, you need to expand your solution, it's too concentrated, you're right.

Scott
 
Hello Butcher,
Assuming my gold has cemented to the remaining copper and silver, will it still drop? If not, should I filter most of the liquid away ( assuming cemented matl. won't pass through filters) allow complete evaporation, then start over correctly? If I were to evaporate the AR is there any possibility solution gold would evaporate away also?
 
let me pass along something that was taught to me. every time you filter either solution or solids, you will leave values in the filter. when ever you transfer values from one container to another, whether in solution or solids, you will leave values behind. start in the container you intend to finish the process in. do not filter unless absolutely necessary. draw off solutions or siphon. leave materials in the container until you are ready to drop the values or all the values need to be transferred to finish a process. understand what to expect before you start the process. what equipment will you need? what does the reaction look like when its happening? what should the solution look like? what should any material left look like? how to tell when a process is near completion. how to test for values. learn these things first and the rest is alot easier.
 
I would do as Hokes suggests add a few drops of concentrated sulfuric to the solution you are evaporating down, this will help keep salts from forming, when you evaporate a little too far, it will also help to make the lead insoluble as lead sulfate.

It sounds like you have a lot of base metals in solution, If you had gold undissolved when you finished the reaction earlier, I would guess you probably used up most of the nitric in solution dissolving base metals earlier, It will not hurt to complete the evaporation process, when you finish it and dilute the solution I would let it sit overnight, and test it with the stannous chloride solution to see if you have any gold in solution.

howdee500,
I really feel you are going about this all backwards, I would study first and get a good understanding of what to do, learning how to do it, before trying to process, by trying to process first, you are not learning how to do it right, all you are learning is how not to do it, and trying to learn how not to loose too much gold in the process, or recover what you have from a mess.

Believe it or not it actually is faster and easier to learn by spending the time needed, by studying how to fly an airplane, before you try it, than it does just to climb into the cockpit, get thousands of feet into the air, and hope you can land that sucker safely, then if you do have to bail out of that plane, you will still need to go back and study to do it right next time anyway.

I do not think I would have tried to remove the nitric with evaporation, thinking I would be able to precipitate gold from that solution.

I would have, probably Just let everything settle, decanted liquid,filtered the liquid, and cemented any values from the solution on copper (if anything besides base metals was in the solution), tested solution to be sure cementing process was complete,decant and treated the solution for waste before disposal, saved all of the material what did not dissolve and any pins or gold fill that was left, separated anything that was not the karat gold, from the karat material, put them in jars and labeled them,the powers I would but with the lower value scrap, and then I would go back to studying Hokes book, to learn how to do it right before I tried again.
 
Butcher,
Had I known of Hoke before starting I would have read until I was comfortable with the process first. This is over 1k of scrap and I'm not rich. The problem is , several sites processes start with AR. One did mention a nitrate 50/50 solution but as written I mistakenly took it to mean that it was only necessary for computer scrap, (desolving board pieces and such) my error. I have since read much of Hoke twice, save osmonium, irridium etc.. but missed the part about how to fix a screw up like I have. I will reread again before proceeding. Be assured before the next batch, I'll know enough.

In the meantime I must know, is there any danger of solution gold evaporating over time, of will it simply concentrate further? Is it best kept sealed or with a cloth cover?

I want to thank you, Scott and any other members for your assistance in helping me to correct my mess and welcome any further suggestions anyone has.
Howard
 
the gold will not evaporate. such solutions may change colors over time, maybe something pricipitating. but the gold will stay in the vessel. i would sometimes check, if there builds a pressure. acid vapors will by the way likely let everyting of iron around oxidise, also if sealed. be sure there will notbuildup a pressure before sealing, if seal at all!
 
Howard,
Gold can be kept in solution and stored, if gold is in solution it will stay there even if you allowed the acids to evaporate off, this is one way a scientist hid his gold from the German Nazis, he kept his gold in plain sight in his lab on the shelf throughout the war, this way when the Germans searched his lab they could look right at the bottle of yellow liquid sitting in the lab on the shelf with the other chemicals, they did not think it was valuable gold in solution, after the war the gold was precipitated and a noble prize medal was formed with that same gold.

If you did store it this way I would use a glass bottle with a glass cork, mainly because if you have free acid in solution, it could change temperatures and want to try to gas off, this would not be a problem if the solution had no free acid and was diluted somewhat, you may get by storing it in an bottle made for nitric acid, or an HDPE plastic bottle as long as it was not for a very long time, and as stated earlier free acid was not a problem, you could check it on a hot day by loosening the cap to see if the heat is building pressure or not from gases (free acids decomposing).

Another tip do the getting acquainted experiments in Hokes book these are very helpful learning tools, they will teach you many very valuable lessons.

Also study the forum which will have many tips Hokes does not cover, like how to use only the amount of nitric acid needed, how you can remove free nitric acid from aqua regia with a gold button, using sulfamic acid to destroy the free nitric acid in solution, some topics like getting your gold pure and shinning and Harold's washing procedures found in the help needed section, and many other things that can add to what you learn in Hokes book.

also when studying Hokes book you have to kind of sit back and also look at the whole picture of what she is doing, do not just read the words and get so caught up in just the part you are reading, like how she separates materials and prepares them before they ever see acids, giving them pretreatments to improve the quality, like incinerating oils or trash, or in quartering the gold with silver and making shot, and then begins to remove base metals from the gold, but does not put gold into solution, so that when she does dissolve the gold most of the other metals have been removed as much as possible...

I also suggest keeping a note book, there is going to be a lot of things you will be learning, small important details if missed can cause big problems, your notes may change some as you learn, so unless you want to be like me, and have to rewrite years of notes in your note book, make your note book where you can add or remove pages or information easily, as you learn more or different details.

I would forget what you have read on the internet, until you understand how to recover or refine, most of the information out there is lacking detail or can be very misleading, some of it is just plain wrong or dangerous.

It does take some time to learn, and a big part of this work is learning to be patient (at least it has been for me), but I have learned that being patient and taking the time to study does pay off in the end.

Howard I think you changing your direction and studying first you will be melting some very pure gold soon, instead of wasting time trying to get out of messes, and trying find out where all the gold you dissolved was going.
I have faith you will do good in this after the learning curve.
 
along with all the other warnings and as long as you are working safely outside or in a fume hood, i will give you a starting point on how to clean up this mess. after you have done more study and understand why it didnt work, this is how i would begin. take what you have now and separate any solids from the solution. filter the solution and rinse the filter. wash any solids back into the solids. keep the solids for later. place a heavy piece of copper (if you use pipe, beat it flat with a hammer) in solution to cement any values from solution. it may take up to a week (time to study). when this time has passed, pull the copper and brush any powder stuck on the copper back into the solution with a soft brush. place the copper back in the solution to rinse any loose powder off. allow the powder to settle until the solution is clear.draw off or siphon the solution from the powder.rinse with water and allow to settle.draw or siphon the rinse from the powder.repeat rinse until the water stays clear. dry the powder and incinerate. boil the incinerated powder in hcl until the solution turns dark.draw off or siphon the solution from the powder.repeat until the solution stays clear. repeat the water rinse until the water stays clear. dissolve the powders with your choice of chemicals (i recommend hcl/Cl and avoid nitric at this stage). if you use hcl/Cl, heat until steaming for about 20 minutes and remove from heat. allow to cool and precipitate the gold.
 

Latest posts

Back
Top