First Mistakes

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lysdexic said:
I'm just checking I don't need gloves right? Copper chloride solution can't be good for your hands or any other part of your body. If I were that stupid with some of the other processes ...well we know what could happen.
I'm not actually sure whether you're being serious or joking. I wouldn't like the stuff to contact my skin at all. I generally wear nitrile gloves until I am working with water. Though I admit to the odd bit of handling without. AP will take off skin pretty darned quick.

I'm a little confused and I don't mean to sound like someone who knows what they are doing because I'm not. I'm just barely to the point where I just might be able to pursue being a beginner, not even an apprentice. You're processing waste acid with copper to cement values there's SMB and possibly Nitrates along with a black powder precipitate? Is this left over poor man's nitric (edit... I meant poor man's AR) that you dissolved gold in? Was it tested? Did any gold drop? Does free sodium nitrate mean there's still nitric acid that should be neutralized before gold can be dropped? I haven't really looked into the process because I don't plan on using it. I purchased 5 gal. of battery fluid (35%? {would have to go look} sulfuric acid) and intend to concentrate it to 98% and use Steve's formula for cold nitric which I plan to distill afterwards. That's still beyond my currant capabilities, so it'll be a while.
Yes. Yes. No. Yes. Yes.

I didn't have stannous at the time, but copious SMB dropped my brown powder. Then a possum dropped my brown powder. I assumed the waste was now gold free, but after some wash-diluting, black stuff dropped a week later. Probably some nitrate evaporated? Reading here made me realise there might be more gold, I added copper. No more powder, yet, but I have enough acid in my jar to slowly get rid of a sensibly priced car.
Adding sodium nitrate (made from ammonium nitrate, thank you Nurdrage - I might be able to cut out the middle man in future??) to HCl will make a weak salty nitric. There's still probably enough nitrate to not drop any more gold despite the masses of SMB, and there's certainly enough of either to confuse my stannous tests. Even my nice, cleanest (SMB still free) "yellow stuff" makes for a purpley-brown test. I'm not touching it until I get the nitrate out. It's just sitting under a clear seedling cover on the front deck in the sun for now. I hope sunlight doesn't screw with it. My "light green stuff", which I know has gold "with a hint of copper", because I put some in and didn't take any out, does not give a stannous result. Probably because of the nitrate.
 
Jason,

I was being sarcastic about not using gloves while handling copper chloride solution. I'm sorry I didn't make that absolutely clear. ANYONE could do a "surf by" and come to the conclusion that I knew what I was doing and personal protective equipment wasn't REQUIRED. It is! It's not just the danger of having flesh dissolved, many chemicals can be absorbed through the skin. I consider that possible with any and every chemical, solution and what not. When I look at what's known now compared to what was known when I took high school chemistry (the mid 70s), who knows what will be discovered in the next 10 - 20 years. When Hoke wrote "the book", tasting solutions to see if there was a sour taste was considered acceptable. Tasting is most definitely NOT SAFE. Handling containers of solutions without gloves is not safe. There is always the risk of a splash as well, so eye protection at the very least. I don't use my oxy-fuel torch without gloves, shaded glasses and non-synthetic clothing. If donning PPE (personal protective equipment) isn't the very first thing I do then I have no business doing it.

It's not really funny but I did laugh a bit about the possum, I always have to take wildlife into consideration. I could run into anything from bear and moose down to a skunk or weasel at any given time. Protect the values and safeguard the poisons.

I decided to take the black powder that dropped from my botched AP leach (that tests negative for PMs) and attempt to digest it with HCl/bleach. I got a greenish yellow solution, thinking gold and copper. I let it sit over night. I'm going to test it this morning. I see why everyone hates tin, that's seems like the culprit. I was able to bring the fouled copper chloride back to life. As long as I can do that I'm going to let it work on waste copper (valueless circuit boards, the pins that had only a few flakes of gold left) until it's completely saturated. I thought Hoke only put PGM containing wastes in the stock pot, but it seems everyone here does or did what my thoughts were and put all PM bearing wastes in the stock pot. I'm thinking any more black powder I recover should get a HCl was and start my stock pot. Time for testing (with PPE donned), errands and more reading. Vacation is over back to work tonight :( Best of luck Jason, we'll get there, all the answers are here just have to recover them and refine them.

Doug

edit - added missing parentheses
 
Safety needs to be everywhere. The number 1 thing I harp on with the kids. "Why do we put all sharp knives in the right side point facing away in the sink before filling with soapy water for dishes?" "Why don't we just reach and grab dishes with glasses in soapy water?" Both will severly cut you. From dish washing to lifting and carrying anything. Always think safety...

The stock pot...
It is not just for recovering PMs still in solution...
It is for rendering all solutions to inert liquids and solids. Envirenmentally safe.

My first stock pot has copper metal in it at all times to drop any PMs.
Then, it is on to the copper dropping pot...Has steel in it.
After that, evaporate and raise PH to begin dropping everything.

Now so far, I have only used HCL, bleach, & peroxide so like acids go in the first.
When I start to use nitric, I will have another stock pot for AR related solutions. Slightly different in solutions as it could dissolve PMs if not properly rendered.

B.S.
...Worst dangers are the ones you overlook...
 
Thank you Pantherlikher. I'm a big boy now and don't have someone standing behind me to slap me up side the head or give me a swift kick in the seat when I really need one. It's all my responsibility. I don't take a disregard for safety lightly even if I had appeared to. Thanks again for the reminder, I personally believe a much harsher chewing out would be in order is in order for me being such an idiot.

Ok... I had an idea and not sure how well it will go over. Where Jason and I are a couple of Noobs going through similar screw ups and all the answers are all ready here... this would be a good place for posting the links to topics where the "big dogs" (I mean that in a most respectful manner) have already explained "it" for the 100th time. Seeing how stock pot was my currant research item and Pantherlikher just brought it up (Thank you) here's my first "gold foil":

cementing the stock pot
http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=49&t=10231

I believe specific posts can be linked to, but why not read through entire topics? I always find more than a quick simple answer as I read through a topic.

Doug
 
Back to cleaning up my mess:

I had over a gallon of CuCl etching solution that was left over from my semi botched attempt at leaching gold plated pins and gold plated circuit boards (there was some solder so it has SnCl in the solution as well). I ended up with a "dirty" CuCl solution from using HCl to remove components I couldn't remove mechanically from some cell boards (not sure what I did to create CuCl but I did and like an idiot I combined that CuCl + "mystery base metals" with leftover CuCl leach solution). I know in the process(es) I dissolved gold (I saw it and into solution is the only place it could have gone). I had a negative for gold with a stannus test (later on I got a faint purple... maybe I screwed up the test I don't know for certain). So that is the origin of my gallon + of CuCl solution.

I took a length of heavy walled 1 1/4" copper pipe and cut up the length with a cut off wheel, cut it into 6" pieces, flattened them into sheets and hung them in my CuCl solution. A little more than 24hrs later the copper was covered with grayish white powder (I figured it was Cu1Cl, researching suggested that was most likely correct) I poured off the liquid until I saw the gray starting to reach the stream and then filtered the remainder of the liquid. I rinsed all of the powder into another container and added some HCl. As expected it turned a light green (darker today). There is some black sediment and still a little gray, but my bubbler is busy and I have some "clean" CuCl leach I want to test and drop any values and combine them (if any) so I can process it all at once.

I'm going to set my contaminated leach aside and save it for removing copper from depopulated boards in the future. I kind of got distracted when I saw my daughters abandoned "potato launcher" (not allowed to call it a cannon at school) she made back in high school for a project. So I stole the 4" pvc necked down to 2" section, cut the 4" section to about 4" long and the 2" section to just long enough for a 2" - 1 1/2" reducer that had been under my feet (literally) and cut a short length of 1 1/2" pvc to finish off the buchner funnel body. I deburred all the pieces now just have to make the strainer. I have some cone type coffee filters that are far better quality than basket type coffee, they have exactly the right area away from the seams to make 4" circular filters and I have an old food saver vacuum sealer that is going to have it's vacuum pump re-purposed. I just need to test a 5g pail to see if it can handle the vacuum. If it works it would make live easier.
 
Sounds like you have a plan...Great.
Try to let as much sediment settle as you can and pour off as much liquid as possible. Then rinse the sediment lots of times with water. Then process the sediment. Filtering is a pain and is not needed for the most part. Filter all liquid off the sediment and all liquids from this point just because...

B.S.
 
Pantherlikher,

Thank you. I did let everything settle for at least 48 hrs, it will be sitting for at least a week before I touch it again. It's a real bear trying to pour liquid off really fine powders, no matter how careful I try to be I always stir the powder up as I near the bottom. I've read a bit about this problem... going to research it more and probably come up with some sort of siphoning system to remove the bulk of larger volume solutions in the future. The whole letting things settle, decant or siphon instead of filtering didn't sink in until I actually tried this. It's not difficult to imagine having half of whatever values were present trapped in a pile of dirty filter paper with whatever other sediment was present and the other half sitting in rinse water from washing it off the filter paper. Right back to where I started with only half the material waiting to settle again.

Pantherlikher said:
Filter all liquid off the sediment and all liquids from this point just because...

B.S.

Because I've reached the point where any values would be in in the concentrate remaining and care must be taken not to lose any?

I still have the cleaner CuCl solution to saturate with copper and collect any values I may have lost there as well. I'll proceed when I've added whatever comes from that batch to the first batch and it has all settled. Where I used HCl to remove the Cu1Cl should I just use water washes before processing? Should I use hot water to remove any lead chloride that could be there? and Harold's wash process using water NaOH water is used for the brown gold powder that is precipitated as the end product of processing? (I'll have to read it again before using it).

My funnel project and I have an idea about making a diaphragm air/vacuum pump are great distractions for (literally) letting things settle. I also made an extended nozzle for my pump spray bottle. It's a pain trying to spray the bottom of a container and I have about 2 doz spray heads and bottles so I tore 2 apart and made an extended nozzle spray bottle. Needs some tweaking but it does work. I'm sure they sell things like that but free and making it myself is cheap and fun.

Thanks again,

Doug
 
Pouring off (decanting) doesn't work well on light powders which are easily stirred up. I never decanted unless the material was heavy. Siphoning works better on most things. You can't remove all the liquid but you can get close on most everything that has settled, whether light or heavy. Before I let it settle, I stirred the solution, put the container on a bench about 3' high, and then tilt the container towards me and put a block on wood under the back of the container, in order to let it settle while tilted. That way, everything settles in a pile at the front. This makes siphoning easier and more efficient.

For siphoning, I used a 5/16" ID clear plastic tubing for 5 gallon buckets and about 3/16" ID tubing for 4 liter beakers. The undesirable curl (from being wrapped around a reel at the store) makes siphoning difficult, but the curl can be permanently removed from the tubing by soaking it in a pot of hot water on the stove for a few minutes, until the tubing becomes cloudy, and then quickly hanging it up for an hour or so with a weight attached to the bottom.
 
Wow, thank you Goldsilverpro. I would have never thought of tilting the container and letting the sediment settle in one place instead of evenly across the entire bottom, or taking the curl in the hose out like that. I know you've done it enough times for me to go with your tubing sizes too. Did you run the tubing straight down the side? About how close to the material did you place the tubing? I hope you don't mind me asking. You already saved me who knows how many attempts at getting it right, if I can increase my odds of success at first attempt why not try? Thank you again.

Doug
 
A little more on taking the curl out of the tubing. Before coiling it in the pot of hot water, I tie a piece of string tightly to each end of the tubing, leaving a small loop for hanging. I hang the top loop on a nail and on the bottom loop, I hang something heavy, like a claw hammer, to stretch it straight. After it has completely cooled, I cut a short piece off of each end to eliminate the kinks where the strings were attached.

I usually paint about 1" of one tubing end with a red magic marker (this has to be renewed every so often) and let it dry well before using. That way I can see how deep it is in the solution. This works well as a depth guide, especially with dark solutions, and it also helps prevent pulling the hose out too far and losing the siphon. I place the tip of the tubing, at about a 45 degree angle, against the inside front of the container and constantly slide it down as the volume goes down. I do it so the red tip is always in view. I do the entire siphoning holding the tubing in my right hand (I'm right handed) 3 or 4 inches from the tip. As the solution level gets near the solids, I gently tilt the container towards me a little more with my left hand. When I see the solids start being drawn to the tip of the tubing, I pull it out. I always clamp one of those cheap ($7 at Walmart) aluminum work lights a couple of feet above the container so I can better see what is happening inside.

With 5/16" tubing, it takes about 5 minutes, or a little less, to drain a 5 gal. bucket. You might try 3/8" to go a little faster but, if the tubing is too large, it can create turbulence and this can stir up the solids. Holding the tubing for 5 minutes can get very tiring. To alleviate this and to make my hand steadier, I rest my right wrist on the edge of the bucket. Right before I start siphoning, I rinse (squirt bottle) and then wipe dry the top bucket edge to remove any chemicals that might eat into my wrist.

I've done this so much that I usually do it without gloves, to maintain a better feel, without getting anything on my hands. I do, however, strongly suggest that you use gloves. Preferably thin surgeon type gloves. Heavy gloves tend to make it more awkward.
 
I will use siphoning, or a chemical resistant chemical pump on larger volumes of solution, like during waste treatment, speaking of waste treatment using the cloth wicking method for sludge is another great tip I learned from GSP.

For decanting solutions I use these tools, the suction bulb pictured is very chemical resistant, I use it on most all of the acid solutions, you can move quite a bit of liquid in a fairly short time with it, cutting the bulb off of one of the pipettes, the pipettes stem tube will fit onto the suction bulb, this gives a longer reach down into vessels, and the smaller opening of the pipette tube creates less disturbance of the settled powders when getting close to them, with these tools you can get very close to the last drop of liquid without disturbing or picking up the powders, the pipette can be used alone, and also serves many useful purposes in the lab work we do, the suction bulb can also be used to start siphoning when using tubing to siphon solutions.

These tools have several uses, decanting solutions, transferring solutions from one vessel to another, removing a bug from solution, adding small amounts of acids to a solution, dripping a drop of reagent into a spot plate...

I have several of these, I will have some of these tools that are dedicated for certain jobs, the old ones go to use in treating dirty solutions, new clean ones will be dedicated to certain procedures like working with clean gold solutions, although they can be washed, to keep from contaminating one solution with another it is a good practice to dedicate these tools to certain jobs, especially were a salt of one solution may contaminate a clean solution.

Note: the suction bulb is not the turkey baster you will find in grocery stores, the turkey basters bulbs are not very chemical resistant, the opening in the end of them is too large and allows dripping of liquids, these suction bulbs I use do not pose these problems.
 

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I can get the pipettes in a 500 count for thirty dollars US. Ebay is a good place to get a few in a pinch.
 
I have used all sorts of rubber bulb pipets for tiny quantities but most of my stuff was in buckets and 55 gallon drums and I found siphoning was much faster and gave better control. I also siphoned most of the solutions in 1 liter, or larger, beakers, tilted, of course, with small tubing 3/16" or less.

Another trick, when removing liquids from settled solids in open top plastic drums when they are sitting on the floor (tilted with a 12" piece of 4X4 wood). I usually just hung a siphon hose (about 3/4" - 1" ID) a little more than halfway down into the solution and let it siphon into another drum until it stopped siphoning (when the solution levels in the two drums are equal). I then dipped out the rest with a scoop made from a 1 gallon round plastic jug. In use, i grabbed the handle with all 4 fingers and squeezed a bit with my thumb on the top of the reinforcing ring. The round jugs work much better than a square milk jug. I held the scoop horizontally flat and slowly pressed it straight down while slightly tilting it, to fill it. I then tilted it up slowly while removing it. With practice, the solids won't be disturbed until you get very close to them and you can drain half a drum in about 15 minutes. See the scoop photo below.

Much of my siphoning was done to make filtering go faster. This was usually when the values were in the solution and the solids were dirt, etc. I let the solids settle and then siphoned off the solution, leaving the dirt in the bucket. I then filtered the relatively clear siphoned solution. This usually goes fast if the solids had been fairly well settled. After all the solution ran through the filter, I then filtered the solids in the same filter paper. This can be as much as 10X faster than trying to filter a whole bucket full of solution with unsettled solids.

Speaking of filtering, except for a few certain things, I prefer gravity filtering to vacuum filtering. In my refinery, I usually had at least 10-15 clean buckets set up for filtering. On top of each, I used fairly large plastic funnels sitting on a piece of plywood with a hole cut in it large enough so that the funnel sat in it about halfway. If the holes are cut accurately, this makes it quite stable and also makes it easy to switch the plywood and funnel to another bucket when necessary without losing any drips. When filtering most things, the solution won't start coming through perfectly clear until the filter paper slightly clogs. At first, I lift up the plywood often and look and the tip of the funnel to check the clarity of what is coming out. When I see it's dripping clear, I switch the plywood and funnel to a clean bucket and re-filter whatever is in the 1st bucket.

This final hint probably sounds stupid but it really works for not losing drips when transferring the filter to another bucket, if you move fast enough. When the filter has slowed to a drip, and the solution is about halfway down, and I want to switch it to another bucket, I pick up the plywood and bob it up and down slightly. Then, immediately after a drip, I bob it up and, at the same time, I move it to another bucket. For some reason, this slows the next drip. Believe it or not.

Here's a typical scoop I made for dipping. It was made from one of those round gallon jugs that you fill with that nasty stuff that you drink before a colonoscopy. Most of the other 100, or so, I have made were from heavy duty round plastic lab jugs. I sketched it out with a marker and then cut it with my pocket knife. Took about 10 minutes, total. Also, it shows how I hold it. Of course, I use gloves when dipping chemicals.
 

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I buy a store brand turkey baster and cut the bulb off of a pipette. I pull the bulb off the turkey baster and drop the pipette,small end first,down through the baster so the small end of the pipette sticks out the small end of the baster. Take hold of the pipette and pull it through leaving just the flared end of the pipette inside the baster.Replace the baster bulb.I put a small zip-tie around the bulb where it connects for an airtight seal.This is for very delicate liquid extraction. I use a different baster with no pipette for moving liquids in a hurry. Like Chris said, in large volumes, it would be best to siphon.
 
I get the suction bulbs from a local pharmacy.

I made a quick Google search of suction bulb images, and found the proper name bulb suction syringe. Here is one place that sells them, you may find them other places also, I just find this tool so handy I had to say something, I also pay very close attention to tricks shared by GSP and others, sometimes the small tricks or tips can make a big difference in making things easier.

http://www.keyhostnet.com/safetynett5/index.php?route=product/product&product_id=92
 
Thank you all very much I wrote a reply yesterday (somewhat lengthy) and my computer froze. I was so tired I was pretty "dungy". In short... I will keep all of what was said in my tool box and I'm extremely grateful to gain the wisdom of much experience first hand for FREE! I ran into a topic I had been trying to find again for a long time today (I wasn't smart enough to bookmark it):

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=325&hilit=getting+gold+pure+shining

There's more than 2 lifetimes of experience just on the first page! In no way do I mean disrespect for anyone when I say there are two people (I am aware of that were very successful professional refiners) here that I pay close attention to when it comes to the actual refining GSP and Harold. I've read where Harold said a number of times how he hasn't had much experience with the escrap refining that dominates the forum. But in my opinion that is only true concerning the initial stage of recovery and not so true once dealing with the "rough" concentrates produced from that initial recovery.

I will probably never even recover what those two did in a single run... The process is the same as it has always been, reinventing the wheel as I've heard said is futile. Adapting the wheel to a specific purpose on the other hand is common sense, meaning tweaking what Hoke taught so that it works best in each situation. When I deal with larger volumes I'll have GSP's tips tricks and hints (the funnel hint isn't stupid... I've used that with pasta for many years). My solutions holding values and my 1/2 pint jar(s) with precipitated gols (and other PMs) butcher's (and Geo's) pipette and bulb syringe will be better suited for the task.

Not used to working 4 10hr night shifts so again I'm pretty much stupid tired right now, but I wanted to say thank you... so Thank you again.

Doug
 
I've found that using a 60ml syringe with a catheter tip is just perfect. You can go as slowly as you like. Something like this, I just happened to have hanging around.
terumo%2060ml%20catheter%20tip-500x500.jpg
 
gsp:
This final hint probably sounds stupid but it really works for not losing drips when transferring the filter to another bucket, if you move fast enough. When the filter has slowed to a drip, and the solution is about halfway down, and I want to switch it to another bucket, I pick up the plywood and bob it up and down slightly. Then, immediately after a drip, I bob it up and, at the same time, I move it to another bucket. For some reason, this slows the next drip. Believe it or not.

If I understand you right, this is the same way I do and the explanation is, I think, you basicly use a virtual zero gravity like in the trajectory for zero gravity maneuver of a NASA training flight.
 

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