Urea is not KNO3, right?

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livinthedream said:
Excellent. think I'm gonna have to buy GSP's book based on the contents I read since this is fun as heck, and I have a limited supply of the current material I'm processing. Looks like there may be info on where the nonpro could inquire to obtain more material. (Hopefully?) I am in the semicon industry, but most stuff seems to be going to solar cell fab these days, other than Intel, AMD, etc. All the generic IC's are fab'd overseas anymmore. (China, etc,) "Political statement entered here" .
Anyway, I must confess it appears I've not studied thoroughly enough and maybe gotten myself into the trap of the beginner. I've not done any inquartation if I'm understanding the meaning properly... mostly due to the idea that I thought AR would be a bit more selective to PGM's than it's appearing to be. As a side note, I do not care about purity in the end either. I will be taking the values I've dropped out to (someone like you guys?) to be assayed. They melt it, assay, while molten, then pay based on the weight and assay % Au.
My values are currently in AR, and I may have been overly optimistic in thinkiing the other metals are insignificant. Turns out a couple of the substrates were alloys of Al, Ti, and Ni, and many may have used Pt as an adhesion layer. The sol'n is now a bubbling murky green (good news, the parylene doesn't seem to be reacting). Hopefully this is normal AgCl I'm thinking. It's going to be difficult to separate the AgCl from all the broken up wafer pieces I fear, but The Ag should be minimal, so if you all think there's 'not enough Au mixed in with the Ag, I may just sacrifice it to the chemical God's. Based on rough before and after weights, I've got roughly 3oz. dissolved metal in my sol'n based on before and after, but haven't tried to thoroughly rinse wafer pieces yet.
OK, sorry for such a rediculously long post, but this potentially pays for my bride and I's camper expenses this year, so don't want to mess it up. It comes down to this. Can/should I use up the HNO3 with some pure Au, or with some scrap that's about 30% Au, and a mix of other metals? How long would it take one to evaporate 120ml HNO3 from the sol'n without heating it if they didn't?
Lastly, I'm all nervous I'll mess something up... Is there anything readily available I can get from a local that would act as Urea to eat up the nitric. remember, I don't care about final purity,
Thanks again!!

You could find urea:
Local garden store
Hardware store
Farmers CO-OP
Wal-Mart
Home Depot

Found as:
Urea
Mixed fertalizer 13-13-13 pick out the white pellets and use them
 
Harold
livinthedream said:
My values are currently in AR, and I may have been overly optimistic in thinkiing the other metals are insignificant. Turns out a couple of the substrates were alloys of Al, Ti, and Ni, and many may have used Pt as an adhesion layer. The sol'n is now a bubbling murky green (good news, the parylene doesn't seem to be reacting).
It's quite important for you to eliminate base metals before dissolving values. There are exceptions, of course, but if it's at all possible, you're well off to do so. In this case, the talk of Al being present is not good. Aluminum, in solution, presents much the same problems that are encountered with tin. Filtration becomes difficult, often impossible. There are pretreatments that can eliminate the aluminum, which would have proven quite valuable for you.

It's going to be difficult to separate the AgCl from all the broken up wafer pieces I fear, but The Ag should be minimal, so if you all think there's 'not enough Au mixed in with the Ag, I may just sacrifice it to the chemical God's.

All depends on how much you'd like to learn about processing, and if you'd like to know how to recover the silver in such an occasion. Assuming you get serious about processing, the mess can be processed in a furnace, where you'd eliminate the unwanted non-metallic substances in the slag. It would also recover traces of values that would otherwise be discarded. End result is a button of metal that can be processed easier than mixed garbage

Can/should I use up the HNO3 with some pure Au, or with some scrap that's about 30% Au, and a mix of other metals?
What other metals? Do not lose site of the fact that base metals precipitate values by cementation. If you add the wrong material to gold chloride, you'll create a mess that is better not created. If you intend to use gold to consume unused nitric, insure that the gold is of good quality, for two reasons. One of them is to avoid adding yet more garbage to the mix, the other being so you can determine the yield of the given lot of material. Any gold that is added will report in the final weighing, so it's nice to know how much was added.

How long would it take one to evaporate 120ml HNO3 from the sol'n without heating it if they didn't?
That's akin to asking how big is a rock?

Evaporation is not an exact science. Temperature and surface area will play a huge role in how long it takes, plus if you follow the idea that if you go through a give exercise a given number of times, success is assured, you open yourself to disappointment. Eliminating the excess acid isn't all that easy, contrary to the opinion of some folks. Even when consuming by added gold, you must allow the solution ample time at a low heat, to consume the acid, plus you must insure you have an excess of HCl.

Do keep in mind, if you evaporate too quickly, you will lose values to the vapors coming off. That's especially true if you have added metal present and it is actively consuming acid. Two ways to determine if you are running to hot. One of them is to put a cold watch glass on the vessel, and note the color of the condensate. If you see anything but a solution free of color, you are evaporating too quickly. The other method is to examine the vapors coming off, again, looking for traces of color. If you see the slightest discoloration, you are losing values.

Lastly, I'm all nervous I'll mess something up... Is there anything readily available I can get from a local that would act as Urea to eat up the nitric. remember, I don't care about final purity,
I'm the wrong person to talk about urea, or anything similar, assuming there is such a critter. I never used urea in all my years of refining. Didn't care to---having worked out a refining process that was to my satisfaction, and turning out gold of exceptional quality. That was good enough for me, and my customers.

Do not fear losing your values. As long as you don't evaporate too quickly, or so long as you don't discard anything without testing first, even if you can't recover the values by conventional means, they are not lost. When push turns to shove, you can always cement the values using base metals, and start the process anew.

Read Hoke.

Harold
 
All depends on how much you'd like to learn about processing, and if you'd like to know how to recover the silver in such an occasion. Assuming you get serious about processing, the mess can be processed in a furnace, where you'd eliminate the unwanted non-metallic substances in the slag. It would also recover traces of values that would otherwise be discarded. End result is a button of metal that can be processed easier than mixed garbage

I guess it depends on how/whether I'll be able to find sources of material going into the future. For now, I just want to cash this in asap. A furnace would be a failry large investment for myself I suspect, but that would be really cool. No idea how much one would be. All I have now is torch that uses O2.

The Au Ihave is 4 9's. I guess I'll go t his route. I just wanted to make sure I'm not going to end up loosing any of that also because I have some strange chemistry in my sol'n. I'll weigh it first, and just put in excess. Would overnight generally be sufficient time?

That's akin to asking how big is a rock?
that's funny. True I guess. Hopefully my last question isn't in the same realm. the 4 9's I have is not a solid button (lots of small pieces (couple mm in size ea), and I have somewhere between a 3:1 and 4:1 ratio of HCl to nitric.

Remember, this go around, I'm not concerned in having pure precipitate. I just want to make sure all the Au is in it. The buyer will melt it all down, determine the % of Au while molten, and buy based on this. He'll finish refining or whatever he wants to do with it. I'll be happy to drop all the Al, and everything else out as long as all the Au comes with it. I won't have created some type of Au salt that won't drop out using SO2 having done this, correct?
Thanks again everyone!! :p
 
livinthedream said:
I guess it depends on how/whether I'll be able to find sources of material going into the future. For now, I just want to cash this in asap. A furnace would be a failry large investment for myself I suspect, but that would be really cool. No idea how much one would be. All I have now is torch that uses O2.
While the reduction can be done by torch, it's not the recommended practice. The flux required is rather aggressive, and the material should have a sufficient soak time for all of the metals to agglomerate.

The majority of us build our own furnaces. It' not a tough job, but one should have need before attempting the project. It does cost a little if you intend to build one that will endure. Commercial refractory, to me, is a must.

Given your circumstances, unless you intend to pursue further refining, it stands to reason that a furnace is not for you.

The Au Ihave is 4 9's. I guess I'll go t his route. I just wanted to make sure I'm not going to end up loosing any of that also because I have some strange chemistry in my sol'n. I'll weigh it first, and just put in excess.
There's a couple things that might be helpful here. The gold I added was always in a button form, so it could be recovered easily. If you use small bits, there's a small chance you won't recover all of them easily, especially if you have an abundance of nitric in solution. An ounce of nitric has the potential to dissolve a troy ounce of gold, so it should be clear that you may end up with a multitude of tiny bits, or you may even dissolve them totally and still need more.

It is relatively common for a beginner to use way too much acid. The ramifications of excess acid don't sink in until you are the one called upon to expel the excess, plus it's hard for one without experience to identify a solution that is free of nitric. As the level diminishes, reaction becomes quite slow. That would be particularly true if you didn't heat your solution.

Would overnight generally be sufficient time?
I am unable to answer that question unless you heat your solution. If you do, and you don't have too much water present, the solution will react relatively quickly with any added gold, assuming you have free nitric. The best way to address this issue is to insert the gold and continue to heat the solution, covered with a watch glass. If there is nitric present, assuming you have free HCl, you will see the familiar brown fumes forming in the beaker, and bubbles will emanate from the bits of added gold. Once the addition of HCl makes no difference to the performance, you can then remove the watch glass and allow the solution to evaporate. It changes color as it condenses, although with the garbage included with your lot, the color would be hard to predict. I would suggest it would be something like a dark green. It's much easier to work with relatively pure solutions, so you might keep that in mind for future operations. Rule of thumb is to always remove all base metals before dissolving the values. It's not always possible.

Remember, this go around, I'm not concerned in having pure precipitate. I just want to make sure all the Au is in it. The buyer will melt it all down, determine the % of Au while molten, and buy based on this. He'll finish refining or whatever he wants to do with it. I'll be happy to drop all the Al, and everything else out as long as all the Au comes with it. I won't have created some type of Au salt that won't drop out using SO2 having done this, correct?
Most likely, that's correct. The real problem is that when you combine various elements, some of them are very troublesome when in solution. Tin, for example, or aluminum, make filtration very difficult. There are some simple procedures you can follow to minimize, or even eliminate, the problems, however. The other problem is the credibility of the buyer. If you open the door to suggestion that your gold is not of high quality, you can safely assume that it will be far worse than it is. GSP has a favorite saying. The refiner is the last liar. My personal experiences with major refiners is that he is correct. They are, in general, notoriously dishonest in their dealings with low volume customers.

It is for good reason that you should study Hoke, and it is also for good reason that you should begin processing in small increments. The concept remains unchanged when you go to larger volumes, but the processing time is much shorter for small batches. That allows you to make the proper observations and to improve your procedures instead of finding yourself in a huge mess, with a lot of values tied up in something that may require cementation and a start from scratch. That, too, is part of your learning experience, but you are far better served to have such experiences in small dosages, so you don't get discouraged.

Refining is one of the simplest functions you can learn. It is not necessarily reliant on skill, but more so on following strict guidelines. If you pay attention to commonly accepted practice and don't get creative until you have a firm understanding of refining techniques, you should be able to turn out quality that rivals industry.

I understand your position with this lot of values, but for future application, shoot for higher quality. It's not only in your best interest, but you will build a far more respectable reputation with those that matter.

Harold
 
I just love reading this stuff. we are so lucky to have these people spend their valueble time giving, we are blessed and I hope they will be too.
AMEN!!
Thanks so much again. With the smaller volumes I'll likely be dealing with in the future, it'll likely be more interesting also to get as pure as possible. I've already got this money spent in my mind, so... The buyer seems pretty reputable, but I was realizing the other day that I'm at his mercy. What am I going to say, "No, there was more Au weight in there than that." try to prove it. Even if I know I added more pure Au than the "assay" says the weight percent of Au is, what am I going to do, other than say that. Anyway, here's to hoping for decency. I guess I can always walk but then I eat the refining fee.
I'm going to go add my "buttons" and see how this goes. I'm giong to let it sit overnight and heat it tomorrow while I can watch for the brown vapor (gas). I'll keep ya'll posted. Last somewhat off subject question, I assume I can melt the sponge using my O2 torch, but will there be much loss? I hope I'm not pushing your patience. Hopefully I can give back someday also.
-dreamer
 
livinthedream said:
I assume I can melt the sponge using my O2 torch, but will there be much loss?
That, again, is a matter of how well you work, and how clean the gold is. Dirty gold tends to be somewhat reactive, often sending off tiny sparks. Those sparks are tiny bits of your gold. If you melt in a (very) clean area, after melting a substantial amount of gold with a torch, you'll find the area covered with minuscule gold spheres. The dirtier the gold, the more you'll find.

Gold is easily melted with an oxy/acet torch, but you have to use wisdom. Start with a soft flame, so it doesn't blow the fine gold powder out of the melting vessel (which should NOT be a crucible. Torch melting with a crucible is a sure recipe for losing some of your values).

Melt your gold in a small melting dish, which has been properly seasoned. As the surface of the gold begins to fuse, you can move closer with the torch, or even sharpen the flame. You can allow it to solidify in the dish, but you must remove it from the flux coated dish while it's still red hot. If it cools enough for the flux to solidify, it won't release. You can clean the small amount of flux that remains on the gold by a boil in dilute sulfuric, which will also somewhat improve the appearance of your gold.

Given the procedure you're suggesting, I expect it won't be pretty. A little pride in workmanship, along with a few more steps, will have your gold looking like it came from someone that knows how to refine. That builds confidence in your buyer, and lowers his ability to be crooked. Most of them are. Been there, done that, got the T shirt.

Harold
 
well, I'm heating my sol'n now. I think it's much more pure than I had originally feared. After the VERY fine pieces of non Au settled, there's very little of it at the bottom of the beaker, and the sol'n is clear yellow. The stuff in the bottom is very light, and moves with the slightest giggle. I also noted when removing all the substrate material that the Al Ni alloy substrates I was afraid of were still intact. They didn't look like they were attacked at all. I'm more optimistic now going forward. I'll post in a few hours and let ya'll know how it goes. Once any free nitric is used up, considering I may now have a quite pure sol'n, what color can I expect? Also, I wasn't sure how far to boil down before I add the SMB.
Cheers!
 
livinthedream said:
well, I'm heating my sol'n now. I think it's much more pure than I had originally feared. After the VERY fine pieces of non Au settled, there's very little of it at the bottom of the beaker, and the sol'n is clear yellow. The stuff in the bottom is very light, and moves with the slightest giggle. I also noted when removing all the substrate material that the Al Ni alloy substrates I was afraid of were still intact. They didn't look like they were attacked at all.
That doesn't make a lot of sense. Are you sure they're metallic?

considering I may now have a quite pure sol'n, what color can I expect?
The color of the solution just deepens. If it is yellow now, it will move towards orange as it is more an more concentrated, eventually turning red and progressing through a dark brown, depending on how far you take the evaporation process. Do note, however, that if you have iron in solution, it, too, will react (and look) much the same way.

Also, I wasn't sure how far to boil down before I add the SMB.
To insure that you don't get the cart before the horse, here, let me make one thing perfectly clear. BEFORE you attempt to recover your values, the last operation should be filtration. The solution should be filtered until it is free of flocculence, or any solid substances. It will have color, but otherwise should be perfectly clear. Anything less is a sign of contamination that will report in your gold.

As far as how far to boil it down, only you can answer that. By adding gold to consume the unused nitric, assuming you have evaporated until the volume has been reduced, and the color is deeper, and there is no action on the remaining added gold, even after adding a small amount of fresh HCl, you can safely assume the nitric has been consumed.

None of this should be performed by the clock. If you make assumptions that a given time interval is all it takes to accomplish the expected end, you will be wrong more often than you are right. You must learn to make observations, following the guidelines I have provided. As you become familiar with the behavior of your solutions, it will all make sense.

Harold
 
That doesn't make a lot of sense. Are you sure they're metallic
Yes, it's a new patented alloy they're using in biomedical applications now. It's called Nitinal (Ni, Sn, Al, and others I believe. the "others" may not be metallic however?). Interesting stuff. It has a fairly low temp memory, so it can be "wadded up", inserted into the body, then it will unfold to the shape that it was "set" to.

You must learn to make observations, following the guidelines I have provided. As you become familiar with the behavior of your solutions, it will all make sense.
yes, it was veryintersting to see the material that was giving it slight cloudiness floculate and clear the sol'n upon heating. The material is now heavier, black and sitting at the bottom with the remaining unreacted Au. I added 40g and am now going to filter the floculant and left over Au and either evaporate further, or just go ahead and drop the Au that's in sol'n.
I've already learned alot.
I did obtain some Urea, so I think I may add a bit of this after I filer the sol'n just to be sure the nitric is used. I did add HCl and didn't notice further reaction, but since it's my first time, and I solidly fall into the category of amateur, I just feel safer going this route before adding SMB. Again, I'll keep yoiu posted. Thank you sir so much!. I'm completely geeked right now.
 
how easily did it filter? tin and aluminum are hard to filter.
just a few prills of urea to warmed solution can be an indicator of nitric in solution, if nitric they fizz,

if added gold was used to rid nitric at evaporation and reaction on gold stopped even hot in concentrated solution, raising temperature will boil off any remaining NOx gas as any remaining nitric has already reached its maximum azeotropic mix in concentrated solution, and the gold in this hot solution reacted with nitric removing it, if any remaining Nitric it will not stay in solution at higher temperature with fresh HCL.

newbies seem to use way too much nitric, and acid to start with.
 
OK. It is SLOOOOW to filter. Should I keep the filtrate and put it in with the material I'm taking to the buyer? Could it be AgCl? There's only a couple grams of it. I'll probably put it in with the mix since the buyer's melting down and assaying anyway. The black flake is still draining. I collected the sol'n that the filtrate was floating around in in a second beaker once it got low, so I'll process it separate from the large amount.
Once I add the Urea, and it's no longer fizzing, the nitric is out, and all that's left is to drop the Au with SMB, correct? I put a couple little balls of it in the main sol'n and it did fizz, so there is some left. Just want to make sure there's nothing additional I should be weary of since I deviated from the original plan.
The reason I used SO much nitric/acid was because the volume of pieces I needed to strip. I've learned from this process however watering it down to the level I'd have needed would have been sufficient since heating keeps the AR quite reactive. I was also under the impression and told from people who have used AR that it's only active for like 30min. That's FALSE!!! I guess it's exothermic reactivity is maybe about that, but heat that stuff up, and off it goes. I'd imagine it would dissolve Au indefinately if you heated it. Anyway. Interesting.
Almost there! It's kind of like cleaning out the dredge or getting to the bottom of a pan. exciting to see what you finally have! Au fever
 
Oh yeah, thanks Barren Realms for the advice on finding Urea. (if you're still following this post) I found some that was 28% (instead of 13) Urea and picked it out from that. not that I'll need the extra. It was like a 20# bag! enough for a lifetime it would appear.
 
livinthedream said:
Oh yeah, thanks Barren Realms for the advice on finding Urea. (if you're still following this post) I found some that was 28% (instead of 13) Urea and picked it out from that. not that I'll need the extra. It was like a 20# bag! enough for a lifetime it would appear.

Very good. Keep it in a dry area. Prefeably in a sealed plastic container.
 
nice, you're online. I'm curious about the Urea reaction. Got a good link of quick line? Is it just reacting with the Nitric? It's no neutralizing the sol'n, ehh? Any idea what gas is evolved?
THX again!
 
livinthedream said:
The material is now heavier, black and sitting at the bottom with the remaining unreacted Au.

Am I the only one that is troubled by that statement? To me it sounds like cemented gold on the "Nitinal" parts. Have you tested the filtered liquid? Maybe your gold is in the filter with the nitinal parts.

/Göran
 
The slow filtering makes me think tin (or aluminum) in solution these will precipitate your gold in the filter and collect some of it there.
usually if these are in solution other base metals are too.

Urea (NH2)2CO notice the two amines, amines once were distilled from seaweed for boiler water treatment (they smell of ammonia), and the carbonyl compound (CO)

here is a formula for nitric acid and urea
6H + 6NO3 + 5 (NH2)2CO ----> 8N2 (gas) + 5CO2 (gas) + 13H2O (liquid)

so from this our gas is carbon dioxide and nitrogen , but I would think different ratios may produce other forms of these nitrogen and carbon gases and possibly hydrogen gas also.

Also Urea as a fertilizer may have a mixture of other crap I would not want in a solution of pure gold.

Butcher
 
There is something missing from that equation.
What about he red cloud? When you add urea to poor man's AR, you evolve nitrogen oxides that are visible. I don't see them in your formula.
 
read that again

here is a formula for nitric acid and urea
6H + 6NO3 + 5 (NH2)2CO ----> 8N2 (gas) + 5CO2 (gas) + 13H2O (liquid)

so from this our gas is carbon dioxide and nitrogen , but I would think different ratios may produce other forms of these nitrogen and carbon gases and possibly hydrogen gas also.


NO2 and NOx are different forms of nitrogen gases.

there is no way I could write all of the formula someone may get from a batch of poormans somebody mixed with base metals and who knows what.
heck someone could have a highly concentrated nitric and add urea and make the explosive urea-nitrate in solution for all I know.

most likely the metals and nitric was where the red gas came from.
 

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