Urea is not KNO3, right?

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One more quick question. Will the yellow solution (orange really) go clear once all the Au is dropped out. I haen't had time to absorb the last 2 posts. Will write again when I get home. The stuff in the filter only weighs a couple grams. I know for a fact there's at least 36g Au in sol'n. The stuff in the first filter with all the Si wafers and Nitinal never had contact with the 40g I put in the current sol'n that I filtered the black stuff off of. All chemicals are reagent grade. gotta split now. I'll write back soon. Thanks to everyone.
 
OK. I'm back. I've decided to slow down with getting this gold out since I have alot, and it's becoming painfully more obvious that just as everyone warned, the new guy tends to use too much acid. Looks like I'm holding par for the course.
chemist, I noticed the brown NOx's during the metal dissolution, but with the addition of Urea, not much at this point, the gases were most definately white vapor/clear.
I've set aside a small amount in a different container (mostly my rinse, etc.) and am testing on this first since I know I stand to mess up what to me is alot of $$ (6 kids and counting baby!! choo choo). I was more nervous last night since this sample amount took a goodly amount of Urea to stop reacting (by the way butcher, the Urea can be separated from the other stuff. you have to make sure you're getting the right fertilizer. It's certainly not reagent grade. I was hoping just a safety net) not only that, after it stopped fizzing, the sol'n seemed to be "carbonated" when I'd shake it (it'd fizz up again). normal? ehh. proceeded with SMB, again poor man's version (campden tablets) It takes alot more of these than I'd have thunk also. I wasn't happy with the cloudiness of the sol'n, and lack of dark precip. I noticed this am however the smaller bottle I was doing this in has essentially become "Au plated" up to the level of the sol'n (not like the sponge I've seem come out of different sol'n's I've worked with). I wish I had a way to know if I've precip'd all the Au (I don't have SnCl, can save the sol'n till I can obtain some I guess though). As stated earlier, I know I have to get at least 36g since that much dissolved using up excess nitric. Doesn't appear it was enough either. Arghh There it is. I"m not doing much more except separating Urea from sol'n till I know for sure what to do. Not sure I have enough pure Au to finish with original plan, and a little nervous to do so honestly. I totally trust the advice I've been getting, just don't trust myself.
Thanks!
 
I'm having more than just a little trouble with not only you, but anyone that thinks they can refine without knowing where they are in the process.

With all due respect to you, your situation, your family, and anything else that may be relevant, you should have never even thought of dissolving your values until you had a means of testing.

My only advice, now, is for you to stop all this foolishness and get some stannous chloride, so you can make some determinations.

Damn it, would any of us think of putting on blinders and then driving our cars? It's no different from refining blindly, although the consequences may not be as severe.

If you can't afford to lose this batch of gold, it's all the more important for you to be able to test. Until you can, and do, you'll never know if you have all of your gold out of solution, or if it's safe to discard an unknown solution.

Take a break, read Hoke, and get on the stannous chloride bandwagon. Only then can you be assured of what you're doing. You might also investigate the use of ferrous sulfate instead of SMB. It does an adequate (read that "good") job, and isn't expensive. It's all in Hoke.

Harold
 
hmmmm. Thanks butcher! I'll definately do this.
Harold, I have nothing invested in this. It's pure profit. (with the exception of the pure Au (which I paid very little for long ago so it's not budget affecting)). I did say this is alot of $ to me, but I suspect it's alot of $ to all of us. I could afford to pay someone else to do this (which I still will in fact) but I find it interesting and exciting like prospecting. Let's not take this personal now. I'll try to not include personal sentiments in my posts I guess. I'm very appreciative for all the input you've provided. I've discarded nothing, so I'm not in a bad situation.
I'm testing on a very small amount and it seems to be going fine. I'm always unsure the first time I do something (I would think most are). Ever get excited about something and just jump in? Sorry if I"m going on, but I have alot of respect and appreciation for you, so I'm hoping you'll see my side. I had decided last night before reading your post to just slow it down and find the time to read the material I need. really I think once I've concocted some SnCl, I'll be doing quite well. Well, off to the hardware store. I'll post after I test my test sol'n unless something goes wrong with the SnCl fabrication.
Thanks again!!
 
I'm getting more and more turned on to the idea of SO2 for precipiration now. I've seen some info on creating a generator, but don't quite have the complete mental picture yet. I have plenty of S left over from the pyrotechnic days, so good there. a fouintain pump and a bucket, so I think I'm close.
I tested my small test batch with the SnCl2 I made today, and got a black indication. gotta find more info about that. Read Chumbawumba and laser steve's threads so far. SnCl2 seems fine.
 
Noxx said:
Trust me, SO2 precipitation is pure joy.
It served me perfectly well for almost my entire refining career. As long as one can obtain it in a cylinder, I recommend it highly. Don't know how I'd feel about making my own, however. If you haven't lived in an environment where you are subjected to SO2 (I was---I was raised in a smelter town, long before it was not acceptable to discharge SO2 to the atmosphere), you may not understand what you're asking for.

I used ferrous sulfate in the beginning, but preferred the convenience of simply turning a valve. I had my SO2 plumbed directly to my fume hood, so I was never exposed. Wouldn't have it any other way, not after having lived with the damned stuff for years, as a child.

I would still recommend ferrous sulfate for the guy that has an irregular need. It's quite convenient, and easy to use.

Harold
 
livinthedream said:
Harold, I have nothing invested in this. It's pure profit. (with the exception of the pure Au (which I paid very little for long ago so it's not budget affecting)). I did say this is alot of $ to me, but I suspect it's alot of $ to all of us. I could afford to pay someone else to do this (which I still will in fact) but I find it interesting and exciting like prospecting. Let's not take this personal now. snip balance of good stuff
I fully understand being excited over the prospects of recovering, and even refining the values. I, too, started without knowledge at some point in time, and was every bit as excited as you appear to be. That I understand. Not testing I do not.

The point I'm trying to stress is that unless you know where you are with the operation, you have no idea what is required. Testing answers those questions. Further, in order for anyone to give you viable guidance, they, too, must know what your tests reveal.

We have a reader on the board that sees absolutely nothing wrong with running without testing. She has openly said so. She does not consider that running blindly. I know it does. She is also the person that has a huge inventory of solutions, about which she knows exactly nothing. She has no clue if they should be processed for disposal, or if they contain further values. No clue, and apparently is content to operate that way. All I can conclude is that it's different strokes. That would not suit me under any condition.

No testing capability? No problem, so long as you don't rely on input from someone that may know how to proceed. You expect help? Then you must be willing to meet, half way, those of us that offer assistance. You do that by learning how to test.

I can't stress testing enough. No one should even think about dissolving values until they have the necessary testing capability. Thing is---it's not expensive, nor difficult. There's no excuse for not having the ability.

Read Hoke.

Harold
 
livinthedream said:
I'm getting more and more turned on to the idea of SO2 for precipiration now. I've seen some info on creating a generator, but don't quite have the complete mental picture yet.

The sulfurous acid document on my website demonstrates making SO2 with SMB powder and a few pieces of glassware.

Steve
 
Great thanks. I'll check it out. I had a little lecture bottle of SO2 at one point we were going to use for testing different solutions effectiveness of capturing stable sulfur isotopes. We were isolating the sulfur isotopes from rocks and obtain signatures using MS. These were then used to help interpret the paleoclimate during rock/mineral formation. Throw in some stable C and O isotopes, and it was pretty amazing the amount of information you could get from some rocks. continental drift, precipitation amounts, type of ecosystem/vegetation, etc. Anyway, where was I going with that. wish I still had that lecture bottle. never got around to that project. may still be sitting in the fumehood. Oh yes, I do remember bubbling it through some of the sol'n's and preciping Barite, PbS, ZnS, etc. If the Au comes out like that stuff did, I totally understand the pure joy comment. First time I ever saw how reactive a gas actually is with a liquid. We weren't even using an aerator, just bubbling it out of the end of a tube, and man did it go.
I hear you Harold, and see your point. I respect that. I'm learning first hand about testing right now. (maybe a little late, but better then than never)
I did test my little bottle I have that I put a bit or urea in (about 30ml or mostly rinse). I thought I put in excess SMB (campden tablets actually. much rather know I'm working with pure. package doesn't say). Au definately dropped, and the sol'n left over is a bit milky I assumed from excess SMB. I tested with SnCl2, but didn't see any comparable color to steve's posts. It was black (I mixed a couple drops of the sol'n with a couple drops SnCl2. then diluted to see if it was just REALLY dark purple). I see purple is the indicator, but couldn't find in any threads what color it should be if negative. I've been assuming there'd be no color change if negative. Hopefully having some base metals in my sol'n isn't going to make SnCl2 testing impossible. So, going back, I know what the maximum thickness of could have been for these films of Au on my stock material, and based on the average etch rate at said temp, I'm confident I got all the values off the stock. Since I did the AR etch "cold", this could be the reason also the nitinal substrates were still intact. It is a strange alloy, but I remember Harold thinking it odd a metal substrate was still there. I guess this could be a method for minimizing base metal dissolution of you know how thick your film of values is. (assuming your substrates are all open to the AR (not stacked, etc.))
well, this post is getting too darn long. I'm going to check out what Hoke says about SnCL2 in the meantime and Steve's site about SO2.
Cheers!
 
livinthedream said:
Oh yes, I do remember bubbling it through some of the sol'n's and preciping Barite, PbS, ZnS, etc. If the Au comes out like that stuff did, I totally understand the pure joy comment. First time I ever saw how reactive a gas actually is with a liquid. We weren't even using an aerator, just bubbling it out of the end of a tube, and man did it go.
I used SO2 for years, exactly as you suggested. Not so much as a pressure regulator. A valve to regulate flow, and a 3/8" pyrex tube, fire polished on the ends. I'd place the tube within a half inch of the bottom of the cylinder or beaker, and turn on the SO2. Regulated properly, the flow comes as individual bubbles which are totally absorbed by the solution before they rise to the top. It wasn't uncommon for the solution to absorb the gas with little action, then for the entire volume to flash, looking very much like bronze paint.

In all my years of refining, I never got tired of watching gold precipitate. It is, truly, the magic moment of refining.

Harold
 
In all my years of refining, I never got tired of watching gold precipitate. It is, truly, the magic moment of refining
.
NICE!!
OK. I checked out Steve's site and was wondering if anyone's ever done this. My question is whether one could just bubble directly into the AR. The idea for using the train is to catch an acid that may make it through as vapor, but would a little H2SO4 in your AR solution mess it up?
On a second note, after testing my little batch with SnCl2 and getting the instant black result, I was took it as a positive and dumped a bunch of SMB in. I noticed last night that the sol'n wasn't cloudy anymore, and there was a very significant amount of precipitate in the boottom. The precip was black, with some gold coloration mixed in becaue the precip when I swirled the bottle pulled off the "plating" on the inside of the bottle I had mentioned earlier. Curious what people think. I didn't have time to test last night, so I will tonight to see if I get a negative in the remaining sol'n. I'm going to Hoke now, if she doesn't mention what a negative shoiuld look like, I'd appreciate it if someone can let me know. I suspect she will. no big deal. I'm just messing around with this little amount of rinse while I learn cause I gotta do something ;-)
 
livinthedream said:
In all my years of refining, I never got tired of watching gold precipitate. It is, truly, the magic moment of refining
.
NICE!!
OK. I checked out Steve's site and was wondering if anyone's ever done this. My question is whether one could just bubble directly into the AR. The idea for using the train is to catch an acid that may make it through as vapor, but would a little H2SO4 in your AR solution mess it up?
On a second note, after testing my little batch with SnCl2 and getting the instant black result, I was took it as a positive and dumped a bunch of SMB in. I noticed last night that the sol'n wasn't cloudy anymore, and there was a very significant amount of precipitate in the boottom. The precip was black, with some gold coloration mixed in becaue the precip when I swirled the bottle pulled off the "plating" on the inside of the bottle I had mentioned earlier. Curious what people think. I didn't have time to test last night, so I will tonight to see if I get a negative in the remaining sol'n. I'm going to Hoke now, if she doesn't mention what a negative shoiuld look like, I'd appreciate it if someone can let me know. I suspect she will. no big deal. I'm just messing around with this little amount of rinse while I learn cause I gotta do something ;-)
Depending on what you may have in solution, it's hard to say what you'd expect, but if you have nothing present but gold, and all of it has been precipitated, the reaction will be nothing. Nothing at all. The solution being tested doesn't respond, aside from being diluted by the stannous chloride. Any color change is generally an indication of values present. Which ones can be difficult to determine until you are very familiar with the reactions. You do that by making standard solutions and testing them until you are familiar with their appearances.

When you introduce stannous chloride to gold chloride, I believe the reaction you see is colloidal gold being precipitated. With platinum, the reaction can be anywhere from a light orange color though dark brown. Some here say they don't see the brown reaction, but that is, in my opinion, because they have little platinum in solution. When you have a few ounces dissolved, it behaves differently, just as gold does.

I am not familiar with anything else aside from palladium. It is the chameleon in the lab. It can manifest itself in several ways, likely due to the strength and age of the stannous chloride, to say nothing of the level of concentration of the solution. I have experienced palladium tests that were easily confused with gold, although only gold will leave behind a purple stain in the spot plate cavity. You can expect reactions from brown through blue and green with palladium, with reactions made even more confusing when you have a mixture of platinum, palladium and gold. Common for refining wastes from the jeweler's bench, or when processing dental alloys. Best scenario in such a case is to test multiple ways, including using a crystal of ferrous sulfate, to eliminate gold, then to test the remaining solution with stannous chloride. You can also use DMG (dimethylglyoxime) to test for palladium. It responds with a deep canary yellow precipitate, and is also useful in testing for the presence of nickel. It's all in Hoke.

Harold
 
great. Yep, I"ve been reading alot of HOke lately. good stuff. I've been successful at dropping my gold. The ScCl2 tested negative just as you described. I think the original test was such a dark purple it looked black. I just put a ton of SMB in after I saw that, and in the morning, I had ALOT of dark precip at the bottom. I tested the sol'n and not really a reaction. tHERE was a very slight orange which settled relatively quickly. Not unlikely it's seeing Pt or Pd since both are not uncommon adhesion layers under the Au. I filtered, dried and weighed the beautiful bronze precip from the Sol'n (had some flakes of gold also since the "plating" from earlier was rubbed off the sides of the bottle when I swirled the precip still in sol'n). It's pretty rich. I've got over 2g in that 15-20ml. Over a liter left to process!!!! This has been really fun for me. Unfortunately, I've been accumulating these choice wafers that were just being thrown out for years now, so it'll be a while before I can accumulate enough to bother with again. I've enjoyed it so much however, I''m going to see what I can do about finding other sources. I'd actually love to be able to do this for a living. I have alot of black sand cons I may try to process. There's no visible Au left in it, but I read somewhere there can still be Au present in combination with the black minerals. May just be something else fun to experiment with anyway. Any tips on finding sources of material would be great. There's a local dentist in the little town I'm in I thought I'd talk to at least to begin with. You guys have been great.
Harold, I especially appreciate yourhelp. If there's anything I can do to help you out, let me know. I've got a propane O2 torch, and Hoke gives me the impression I can melt the Au with it, so I'll be sure to get a pic for everyone at least. More to come. You guys and this site are amazing!!
Cheers!!
 
forgot to ask, does Hoke discuss the use of SMB to drop the gold. I've only read about her using copperas, which I'd rather now. Ideally, I'll use SO2, but since the SMB worked on my small rinse test, "if it ain't broke...." I know, not a very good phrase since I do want to learn more methods, but for now a good reference on SMB (maybe particularly even campden tablets) would be great.
I guess specifically, Hoke mentions if the excess nitric hasn't been removed, the copperas will do this, you just have to add more. Will SMB tablets do the same thing?
 
livinthedream said:
I filtered, dried and weighed the beautiful bronze precip from the Sol'n
That's good for the moment, but your precipitated gold should be washed. That's true even if the resulting barren solution is colorless. Amazing things are removed by the (proper) washing process.

I'd actually love to be able to do this for a living.
My hobby evolved to just that. It was so successful that I had to close the doors on my commercial machine shop. It can be done, but it happens on it's own schedule.
I might also add, my success came at a time when there was little control on chemicals. I could purchase my needs through my machine shop, with prices that were very reasonable. A 55 gallon drum of HCl cost but $57 back then, and a 55 gallon drum of nitric cost $207. It is much more difficult, today, to make something like this work. That's not to discourage you, but to keep your thinking on an even plane.

The best advice I can offer anyone where refining is concerned is to get established with manufacturing jewelers. They have a constant need for refining, and produce the second best possible scrap on the market, the dental trade being the best.

By making connections with jewelers, you not only create sources of material to refine, but an outlet for pure gold. These people generally pay over spot for pure, so you can offer your refined goods for spot, or even slightly higher, which will be to their, and your, advantage. You will come to understand that selling gold for spot is not easy, but is made much easier when you become recognized as a competent refiner.

I have alot of black sand cons I may try to process. There's no visible Au left in it, but I read somewhere there can still be Au present in combination with the black minerals. May just be something else fun to experiment with anyway.
If nothing else, it will help you understand why black sands are not generally accepted for processing. I expect you'll be wasting your time, but you will gain knowledge, and that comes with a price, so it's worth your time to investigate.

There's a local dentist in the little town I'm in I thought I'd talk to at least to begin with.
The advantage of dental wastes is that they are (or used to be) of much higher quality. They also contain platinum and palladium, so the overall value is much greater than typical jewelry. The problem is, gold is no longer used as it once was, so it is likely not a great source. Still, old dental work is replaced as it wears out, so the old material is still out there. It comprised a small percentage of the refining I did when I was active, often provided by jewelry manufacturers (bench men) who took it in in trade.

Harold, I especially appreciate yourhelp.
Welcome. I hope I have been of some assistance. As you discovered, I have little patience for those that don't pursue refining with some structure. There are no shortcuts, and if you gloss over the operations, it is unreasonable to expect acceptable results. I have all the patience in the world for someone that is trying, following acceptable procedures, but run short in a hurry with those that ignore proper procedures and look for instant gratification. Refining can be very rewarding, but you must do your part in order to achieve success. I believe you see that now.

I've got a propane O2 torch, and Hoke gives me the impression I can melt the Au with it, so I'll be sure to get a pic for everyone at least.
With O2, it will work. It's a tough call without, however.

More to come.
Good! I'll be looking forward to your posts and pictures of your success.

Luck!

Harold
 
Harold_V said:
It has everything to do with how you're refining.

There are NO shortcuts. If you want pure gold, you MUST follow accepted practice. Remember, those that went before us have gone through this time and again----and have perfected a process that will yield good quality------so if you're interested in achieving that level, follow instructions that are at your disposal. Don't experiment-----leave that for others with time on their hands that are content to re-invent the wheel. This is particularly important for you, considering you're trying to establish a refining service.

Depending on what you're starting with, you may have a hard time achieving a good level of purity the first time through. That's to be expected. Part of the problem is mechanical drag-down, where you're working with very heavily contaminated solutions, part of which follow the gold. They're not always easy to wash out, even when boiling with HCL.

My advice to you is this:

Process your gold the first time, using conventional means. Allow as little in the way of contaminations (metals) as is humanely possible, to be included with the gold. Use only clean vessels. Wash them well between operations-----and use BonAmi cleanser if necessary to remove stubborn stains. Do not use other cleansers, for they scratch the glass. Filter before precipitating, and insure that the filter does not allow particulate matter to pass. If it does, re-filter, or go to a better filter grade. A Whatman #2 does an outstanding job for first refined metals, although they are not cheap. I used them exclusively for filtering first run gold chloride. I felt they were worth the extra money. At all times, keep your beaker covered with a watch glass of appropriate size, to prevent contamination from other sources.

Precipitate your gold using conventional methods, collect it and wash it well. It's best to use a precipitant that does not add contamination. I preferred SO2, but there are others that work equally as well, I'm sure.

First wash should be in boiling HCL and tap water. Boil for a prolonged period of time. Take up the solution with tap water, decant after the gold has settled, then rinse with tap water, which should again be brought to a boil. After it has boiled for a period of time, add more tap water to cool the lot, then decant as before. Rinse again, and do it until the wash water comes off clear. Next, wash the gold with ammonium hydroxide and tap water. Heat it until it boils. You'll notice that the solution gets discolored. How much is determined by how dirty your gold was when you started. The ammonia evaporates fairly quickly, so you can't boil very long. Add tap water to cool, decant, and follow up with a tap water rinse, again, boiling the water. Add tap water to cool, then decant. You now repeat the HCL and tap water wash. You'll be amazed that suddenly more contaminants will come off. Boil well, add water to cool, decant, repeat the water rinse, decant, then, and this is important-------start the refining process all over again by dissolving the well washed gold powder in aqua regia. I'll talk about that in a minute, but these are indicators you should have observed along the way, aside from the fact that you could see contaminants being washed from your gold powder.

The gold powder, which started out quite dark, is now much lighter in color.

It may have been rather loose and flocculent, but now is eager to agglomerate, so it forms lumps and settles quickly.

While these instructions sound like a lot of wasted time, when you process what you think is pure gold, you'll see evidence in the remaining solutions that it was not. The evidence of which I speak will be in your solution when you've extracted the gold for a second time. It's a lot of work which is why I re-refined my gold in large lots, often as much as 200 ounces at each refining, so the time spent yielded a large return.

When you precipitate for a second time, one of the things that you can do to help eliminate unwanted elements is to use a different precipitant than the first time. I never bothered with that, but it's good advice if you're fighting with a given contaminant and can't get rid of it by other means. That was never a problem for me.

Wash the gold powder the second refining by the same methods and sequences as the first refining. Make sure all your equipment is scrupulously clean. Force dry the gold when it's washed by heating the beaker at a very low heat for a long period of time. Avoid allowing the beaker to achieve boiling temperature---you get minor steam explosions that blow gold out of the container. As the gold dries, it's a good idea to swish it around the beaker occasionally, which prevents the gold from bonding to the beaker. The residual matter in water tends to form around the gold and bond it to the beaker. While it's a contaminant of sorts, it does NOT alloy with your gold, so it is not a source of lowering the fineness unless you have strange elements in your water. For me, it was not a problem.

Once dry, you can then melt your gold. A clean, never used for anything but pure gold, dish can be used. It should be covered with a coating of borax, but nothing else. DO NOT USE ANY SODA ASH. If there are any oxides present, they'll be reduced and absorbed by the molten gold instead of locked in the flux.

Your torch should be cleaned of loose crud before melting your gold. Run fine abrasive cloth over it until it's very clean, then wipe it down with a damp cloth to remove any traces of dust. Think clean every inch of the operation-----otherwise you undo all the hard work you've done getting your gold pure.

Your other option is to operate a small gold cell, but you must have several ounces of pure gold for the electrolyte.. That is likely not a viable choice for you at this point in time.

Harold
 
WOW, more. working on the HCL wash right now. I found some yellow bits in my filtrate that tested positive for Au. I may not have rinsed the little bit I had REALLY well, but it was VERY positive. Any ideas what this might be? It looks just like S that's been melted. There's not a lot of it, but... Seems to either be H2O soluble or really easy to break up into small enough particles to seem dissolved in the H2O.
 

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