# Drop it like it's Hot (chemistry questions about dropping the gold)



## snoman701 (Mar 28, 2017)

Multiple questions about the drop. 

1) I did two today using SMB. The first...big chunks of gold. The second...slow, fine gold. 

2) What are the situations that produce big chunks vs the fine stuff that takes forever to settle?

3) Also...is dropping with SO2 really as simple as just putting a hose in the beaker and letting it bubble? Does it work on excess nitric as well? 

4) This is so much fun I'm thinking about building an SO2 generator. Is anyone using one? Is it really necessary to bubble the SO2 through concentrated H2SO4...I mean, it's being bubbled in to an aqueous solution. 

5) Finally, does my copperas look right? It wouldn't go in to solution with water, so I added sulfuric acid to it and heated it. It did this really cool boiling thing where the whitish layer would boil underneath the sulfuric acid...then when cooled it did this. The whitish layer SEEMS to be solvent in the water/sulfuric above...if you break in to it and start stirring. (picture is on cell phone, so I have to post this, then post picture)

Both beakers are essentially the same, just two batches.


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## snoman701 (Mar 28, 2017)

Here we are










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## glorycloud (Mar 29, 2017)

Hmmmm. That doesn't look like any gold I have ever seen after an SMB drop.
Did you remove the base metals before the drop? What was your process prior
to the addition of SMB?


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## Topher_osAUrus (Mar 29, 2017)

glorycloud said:


> Hmmmm. That doesn't look like any gold I have ever seen after an SMB drop.
> Did you remove the base metals before the drop? What was your process prior
> to the addition of SMB?




I think thats his "copperas" dissolving, and it doesn't look right.
I kind of see a slight green tinge to the liquid, but, there is something wrong with it... It looks sickly. :lol: 

Where did this copperas come from? By chance, is it anhydrous ferrous sulfate? The good green crystals of copperas have water in their formula.

I would like to see your gold though, too! ...instead of just showing us your gold laden processors :wink:


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## anachronism (Mar 29, 2017)

Ewww what the heck?


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## snoman701 (Mar 29, 2017)

Exactly!!!


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## anachronism (Mar 29, 2017)

Sno I'm going to be politely blunt.

The time to start thinking of building S02 generators, or any other equipment is when you've grasped the basics and understand exactly what's going on in your solutions to the point where you can control a reaction, and drop gold cleanly. Now it takes guts to post up those pics and I take my hat off to you for doing so but now is the time to step away from all the other ideas, all the equipment plans and learn to refine gold from the floor up.

When you've got that, and can do it repeatedly then you can think about other things. 

Typed with the best of intentions

Jon


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## snoman701 (Mar 29, 2017)

Fairly said....appreciate the candor! 

Here's another 2 grams of dirty powder topher. 







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## kernels (Mar 29, 2017)

Yeah, so, I was considering being politely blunt yesterday and luckily Jon beat me to it. 

You appear to have some awesome scrap to process, but at the moment you are wasting it through inexperience. 

Be super careful with Sulfuric and water in the same general area.

As far as your SMB drops - The big chunky stuff that settles fast is a clean solution that is giving you clean gold. The fine crap that takes days to settle is a dirty solution and is going to give you dirty gold. Did you leave the solutions to stand for a day or two before dropping the gold to allow chlorides to settle on the bottom ? Did you add a few drops of Sulfuric to the solution to precipitate out any lead before dropping with SMB ?


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## snoman701 (Mar 29, 2017)

So the copperas that I posted exists like that because that which I ordered was oxidized. It started out all brown. The liquid portion is a mixture of water and 10% or so sulfuric acid. There is a layer that seems to be quality crystals, and I've been digging them out and trying to dissolve them (successfully) and recrystalize them in another dish. As I do this, the layer seems to regenerate some. 

I'm thinking that it's just lacking enough water, but also because it didn't have the right amount of water to begin with, it didn't slowly crystalize out. 

I've been using SMB to drop my gold as of now, which has been working for me. To be flat out honest, I'm still using dirty glassware. I'm still trying to figure out what is best, what volumes are best, what is most comfortable to use, etc. But dishes are pretty difficult as well, being on a well & septic, I don't want ANY of my dishwater going down the drain. I usually pre-wash it in the shop, then only when it seems clean there, will I take it in to the "kitchen" to wash it. 

So there are a lot of things besides myself that are working against me. 

I can't tell you how much I miss my lab...a proper hood, a heavily ventilated room on top of it...and I didn't even have the neighbors trying to figure out what that guy is doing standing outside with a hotplate & lab glass.


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## anachronism (Mar 29, 2017)

Why do you have sulphuric acid present in your copperas?


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## snoman701 (Mar 29, 2017)

kernels said:


> Yeah, so, I was considering being politely blunt yesterday and luckily Jon beat me to it.
> 
> You appear to have some awesome scrap to process, but at the moment you are wasting it through inexperience.
> 
> Be super careful with Sulfuric and water in the same general area.



The sulfuric is "just" battery acid. I haven't been able to find gauntlets locally, so I haven't started using concentrated sulfuric. 

I'm not processing anything "nice" at this time...for the most part. 

Yesterdays gold was the result of me saying "I give up"....so i threw some gold capped cdips in to a beaker and dissolved everything in AR. Up until that point, I wasn't really certain that I had a reasonable quantity of gold in any of my solutions. They tested positive via stannous, but that doesn't mean it's going to be a good drop. That was the first drop that actually dropped. The others have mostly taken cementation. 

When I started, the only gold I had was my wedding ring...and while I have an understanding spouse, she's not THAT understanding....so even working through the basic exercises in Hoke was impossible. I am really just now feeling like I'm getting there....plus, now I've got enough gold that I can do the exercises, and hold myself accountable. The problem with E-scrap is it's soooo variable. 

This powder is the result of my stock pot....where all the previous mistakes went. Added to it was a few assays of some heavily plated copper parts. 

What is shown, is just a drop in the bucket of my nicer stuff. I bust my butt to find this stuff, and I pay for it...but there is enough data on this site that I'm comfortable with the prices I pay, if I'm careful. I figure if I keep my cash price below boardsort, and concentrate on things that are easier to process like ceramic processors, I'll be mostly safe. Plus, if I ever need to cash out, I can just drive it all out to Cleveland and dump it. Though at the rate it's accumulating, I may be better off selling direct to one of the batch processors like SIPI. 



> As far as your SMB drops - The big chunky stuff that settles fast is a clean solution that is giving you clean gold. The fine crap that takes days to settle is a dirty solution and is going to give you dirty gold. Did you leave the solutions to stand for a day or two before dropping the gold to allow chlorides to settle on the bottom ? Did you add a few drops of Sulfuric to the solution to precipitate out any lead before dropping with SMB ?



Thank you! This is the knowledge that I find difficult to locate. So if I've got a clean, balanced solution, I should always see nice grain sizes then...and vise versa, if it's fine ugly gold, it's likely coming from a dirty solution. In this case, this was the first refining of the stock pot AR, and it was dark dark green. 

I let them stand overnight. 

I did not add sulfuric...concentrated or dilute?


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## snoman701 (Mar 29, 2017)

anachronism said:


> Why do you have sulphuric acid present in your copperas?



To reduce the oxidized copperas so that it would again be soluble in water. 

I did this on the small scale...I mixed a couple table spoons of oxidized copperas with sulfuric acid to be around 10% by volume. I then heated and stirred the solution. It all turned the pretty green color. Upon addition of MORE powder, I got that ugly mess. 

Addition: note that the white layer beneath the intermediate layer IS crystallized, it's just not the pretty green crystals. They are more linear. 

The other answer is Butchers statement that leaving the copperas crystals submerged beneath a sulfuric acid layer will keep them from oxidizing.


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## kernels (Mar 29, 2017)

snoman701 said:


> I let them stand overnight.
> 
> I did not add sulfuric...concentrated or dilute?



Excellent, sounds like you are doing better than your top post suggested.

Have you noticed any white powder settling out of your solution when standing overnight ? I find it best to siphon about 3/4 of the solution after any white powder settles for a day or so, the other 1/4 goes into a larger holding bottle where pregnant solution accumulates over time while all the white powders from all the individual batches settle in the bottom of the bottle. I hope this makes sense, Even I find it hard to read!

You want your solution to be 100% crystal clear before you drop with SMB, don't worry about the color too much.

I don't think the concentration of the Sulfuric makes a big difference, but I may be corrected by someone more knowledgeable. I use Sulfamic acid to convert excess Nitric in my solution to Sulfuric. This is usually enough to precipitate any lead, so clean dilute Sulfuric should also work. Add the Sulfuric (or denoxx with Sulfamic) and then let the solution stand for a day.

I haven't tried myself, but read a few times that making copperas from scratch is pretty simple, I believe you just need some iron from the laminations of a transformer and Sulfuric acid. 

Occasionally I still get a dirty drop where the gold does not 'clump' or settle fast. In these cases I leave it to settle for a couple of days, then do a second refine and pay more attention to separating out the clear solution from the settled white / grey powder.


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## snoman701 (Mar 29, 2017)

kernels said:


> Have you noticed any white powder settling out of your solution when standing overnight ? I find it best to siphon about 3/4 of the solution after any white powder settles for a day or so, the other 1/4 goes into a larger holding bottle where pregnant solution accumulates over time while all the white powders from all the individual batches settle in the bottom of the bottle. I hope this makes sense, Even I find it hard to read!


No, not making sense.

Once I have a pregnant solution, I denoxx with sulfamic. I then dilute this to at least two times the volume, adding ice to bring the temperature down. Once the ice is completely melted, I add my SMB, wait about fifteen minutes and test with stannous. If test was negative for gold, I let it sit overnight.

Once it is settled, I pour off (through a filter) supernatant liquid, minding to keep a steady hand and a slow pour to keep the gold from moving. I then wash in distilled water as many times as it takes for me to be confident that it's pretty clean. If I'm using a beaker, that could be three....if a canning jar, as I had to earlier, it was a lot. 

Supernatant liquid is transferred to stock pot to sit. Stock pot is rarely moved from it's place on the bench...I drain by siphoning off all but the last inch. 

The only white powder I remember was when I was still using coffee filters. I attributed it to the glass frit they glued cdip ic's together with...and I could never seem to get it to filter out. Also, silver chloride, which is in a seperate bucket.


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## kernels (Mar 29, 2017)

snoman701 said:


> Once I have a pregnant solution, I denoxx with sulfamic. I then dilute this to at least two times the volume, adding ice to bring the temperature down. Once the ice is completely melted, I add my SMB, wait about fifteen minutes and test with stannous. If test was negative for gold, I let it sit overnight.



OK, so that is likely part of your problem, next time, after denoxxing with Sulfamic let the solution sit overnight before you drop the gold out. There will be a thin layer of white powder sitting on the bottom of your beaker. This is what is contaminating your gold.

What is happening is the Sulfamic is turning excess Nitric into Sulfuric, the Sulfuric is causing lead to precipitate out, but you are then immediately dropping the gold, so your gold powder is full of lead chloride.


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## kernels (Mar 29, 2017)

So, the 'holding bottle' that I was trying to explain before, is just a bottle where the left over pregnant solution and white powder from many individual batches goes after I have siphoned off the top 3/4 of the pregnant solution. The powder settles in the bottom of the bottle and when the bottle starts getting full (usually about once a month), I once again siphon off the pregnant solution leaving some solution and the white powder in the bottle. 

I use a 2L glass bottle for my holding bottle, but you could use any suitable container you have available. The key to not have any fine powder in suspension when you drop the gold. The solution must be 100% Crystal Clear!


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## snoman701 (Mar 29, 2017)

Ok....yeah, I haven't had any problem with clear solutions since I switched to proper filter papers. After I filter it, I use a lot of distilled water to flush the pregnant solution from the filter paper. Then once done, the filter paper goes to my filter "bucket" for an incineration at some point. 

I've been very careful to make sure that I only drop (or cement) clear solutions.

I have a similar bottle that I use for silver chloride. I let it settle, then siphon off excess.


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## kernels (Mar 29, 2017)

Filter papers wont catch the super fine powder, and washing the filter paper after filtering is just helping more of the fine powder make it through the filter. Using very good lab filter paper and a vacuum setup is better than coffee filters, but still no match for waiting a day for the powder to settle.

I keep saying the same thing, but somehow the message is not getting through. Just try leaving a solution sitting for a day after denoxxing (before dropping the gold), you will see the fine layer of sediment settle.

Your solution appears clear, but likely has very fine powder in suspension. Only experience will teach you the difference between a solution that is 100% clear and one that is not.


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## anachronism (Mar 29, 2017)

If you can read a newspaper through it clearly or shine a laser through it clearly then it's clear. 8) 

Whatman number 1 papers will take a solution to crystal clear.


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## snoman701 (Mar 29, 2017)

anachronism said:


> If you can read a newspaper through it clearly or shine a laser through it clearly then it's clear. 8)
> 
> Whatman number 1 papers will take a solution to crystal clear.



I am using a whatman 44 (ashless)....3 um retention. Got them really cheap.


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## snoman701 (Mar 29, 2017)

kernels said:


> I keep saying the same thing, but somehow the message is not getting through. Just try leaving a solution sitting for a day after denoxxing (before dropping the gold), you will see the fine layer of sediment settle.
> 
> Your solution appears clear, but likely has very fine powder in suspension. Only experience will teach you the difference between a solution that is 100% clear and one that is not.



No, it wasn't getting through....sorry. I'll give it a try...


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## anachronism (Mar 29, 2017)

snoman701 said:


> anachronism said:
> 
> 
> > If you can read a newspaper through it clearly or shine a laser through it clearly then it's clear. 8)
> ...



That's better than the ones I use so you should get perfect results- vacuum assisted I assume?


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## kernels (Mar 29, 2017)

snoman701 said:


> kernels said:
> 
> 
> > I keep saying the same thing, but somehow the message is not getting through. Just try leaving a solution sitting for a day after denoxxing (before dropping the gold), you will see the fine layer of sediment settle.
> ...



Now I really hope you see the settled powder, otherwise I will look pretty silly! But it can't hurt to try it anyway. I can just advise the technique that I have found to consistently give me cleaner drops. I am a believer in giving solutions time to settle. 

anachronism - do you need a vacuum setup for the #1 or will clear liquid pass through OK by gravity ?


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## anachronism (Mar 29, 2017)

You need the vacuum if you are using circular filters because it holds the paper down so that no liquid can pass without going through the filter. If the vacuum stops on a buchner the first thing that happens is that particles go through and it's a real pain.


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## kernels (Mar 29, 2017)

Unfortunately my only experience in this matter is that two coffee filters are completely useless at removing the fine (lead chloride ? silver chloride ?) particles. Generally I'm in no rush, so happy to let it settle for a day or two before separating off the clear solution.


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## anachronism (Mar 29, 2017)

kernels said:


> Unfortunately my only experience in this matter is that two coffee filters are completely useless at removing the fine (lead chloride ? silver chloride ?) particles. Generally I'm in no rush, so happy to let it settle for a day or two before separating off the clear solution.



Here's what I used to do before I got he Buchner.

Rough filter using single coffee filters. Then use 2 once, then use three and pass it through the same filters a few times.


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## snoman701 (Mar 29, 2017)

anachronism said:


> You need the vacuum if you are using circular filters because it holds the paper down so that no liquid can pass without going through the filter. If the vacuum stops on a buchner the first thing that happens is that particles go through and it's a real pain.



No, I use a cone funnel, then fold the filter paper in to a cone, and just always make sure I don't pour over the filter.

I'm still using what I get cheap or free....in time I'll decide what I *want* to use. It's clear that I need a good vessel JUST for dropping gold in. New & unscratched! 

I'm not a big fan of the buchner funnels right now. I have them, but I haven't had good consistent vacuum, so I haven't been using them....and, I'd have to cut the papers down to fit, so what's the point. Actually, I haven't used a buchner since I was using coffee filters. I clogged one of them up with the fines that pass through the coffee filter. Not quite sure how to get those out...maybe boil in AR. If that doesn't work, I'll try throwing it in the kiln and annealing it. That's how we used to clean used glassware...just send it to the glassblower. 

I really think my biggest problem with the button I posted is my melting dish. I should photograph it. I bought it at a flea market a long time ago just for the handle. Time will tell.


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## snoman701 (Mar 29, 2017)

kernels said:


> Unfortunately my only experience in this matter is that two coffee filters are completely useless at removing the fine (lead chloride ? silver chloride ?) particles. Generally I'm in no rush, so happy to let it settle for a day or two before separating off the clear solution.



That, I completely agree with! I had the same problem with the coffee filters. It may have been lead or silver, I always assumed it was from the glue holding ic chips together. 

I'd be happy to have it either of those, should make it easy to get the buchners clean!


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## snoman701 (Mar 30, 2017)

kernels said:


> Unfortunately my only experience in this matter is that two coffee filters are completely useless at removing the fine (lead chloride ? silver chloride ?) particles. Generally I'm in no rush, so happy to let it settle for a day or two before separating off the clear solution.




Ok....tried it. No white powder. 

If you'd like to try some "proper" filters, pm me your mailing address. Least I can do. 

No attitude or anything intended btw...I appreciate any and all help. I like knowing other options as well!! 




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## kernels (Mar 30, 2017)

snoman701 said:


> kernels said:
> 
> 
> > Unfortunately my only experience in this matter is that two coffee filters are completely useless at removing the fine (lead chloride ? silver chloride ?) particles. Generally I'm in no rush, so happy to let it settle for a day or two before separating off the clear solution.
> ...



Did the gold drop clean then ?


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## snoman701 (Mar 30, 2017)

Won't know until it settles. It was more brown than black, that's for sure.

If I don't get a clean button on this round, I'll likely have to inquart to rid of pgm's.

Sound like an appropriate plan???


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## Shark (Mar 30, 2017)

As for filtering, I use a charmin plug. It stops fine particles that can slip through common filters.


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## g_axelsson (Mar 31, 2017)

Once I bought proper filter papers I never looked back. The only thing I use coffee filters for today is cemented copper. Anything that slips through there is not worth chasing.

Göran


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## anachronism (Mar 31, 2017)

g_axelsson said:


> Once I bought proper filter papers I never looked back. The only thing I use coffee filters for today is cemented copper. Anything that slips through there is not worth chasing.
> 
> Göran




I use them still for rough filtering large volumes Goran- makes the vacuum filtration later a lot faster when you've got the serious gunk out of the solution. I've used loads this week filtering the Nitric washes on the jewellery slags.

I completely agree though- I remember the first time I used a vacuum setup with proper papers. I nearly cried when I realised how much time I had wasted before. 8)


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## upcyclist (Mar 31, 2017)

I'm in the same boat--the old coffee filters mainly get used for waste processing now. I'll use a couple to filter decanted stockpot solutions, just in case there are floaties with PMs in 'em 

I use #1 or #2 filters (which one depends on how much I care) in a Buchner with a simple hand pump that came with the funnel as a kit. Works great for my level of work.


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## patnor1011 (Mar 31, 2017)

I do use coffee filters when filtering AP solution due to their size and shape which will fit my strainers. For AR or gold chloride solution I do use buchner and proper filter papers which I cut to desired size.


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## snoman701 (Apr 1, 2017)

Spent some time on this this morning.

The copperas, posted above, is the result of not having enough water and too fast of a crystalization.

When I added excess water, 50% of it was immediately soluble. The other 50% needed a little more sulfuric acid to turn clear.

Now it's all occupying all of my crystalization dishes, as well as other dishes in the oven. After that, I'll dissolve it again and do a hot filtration and I should be good to go with it. 

So if you are recrystallizing oxidized copperas, make sure you do so with enough water for it to all dissolve cleanly.


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