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no1special

Well-known member
Joined
Aug 5, 2012
Messages
54
Location
SE MO
If stannous test comes back neg, then no more smb is needed, correct? This is 18g of 14k jewlry that i quartinated then did poor mans AR evaporated down the added hcl, after all corn flakes had disolved. Then I added ice and then filtered 3 times till not murky, added water put on low heat and added 15g of smb. After two hours there is a small amount of powder on bottom, but nowhere near the 10 grams or so that i am expecting. The solution is still very dark as it has been since added smb and the qtip shows a before (positive) and after (neg) stannous tests. Should i leave the heat on or off while i let settle overnight and should it be covered or uncovered with heavy watch glass?
 

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after inquarting and cornflaking, did you digest in nitric acid to remove the silver before you went to AR?
 
yes i did sorry forgot to mention that. Was done with some home made nitric using laser steve's recipie using sodium nitrate and rooto, which seemed to have worked quite well. The silver dissolved and was recovered from blue solution via salt to sodium cloride (i know not recommended, but i had no clean copper and wanted to be sure that it was in there). And the stannous test shown was just prior to, and two hours after adding smb.
 
looks like a colloid in the jar. hard to say what kind. its not recommended to use one pot nitric (poor man's nitric) to dissolve silver. the purple looks like silver chloride thats been exposed to bright light.
 
How does the solution filter, that can be a clue, colloidal solution (from tin will give trouble filtering) if this was karat gold and not gold plated material I would not normally suspect much if any tin here, but you never know.

The color is very dark,it is hard for me to tell what color it really is.
What color was the solution before you added SMB, was it a clear yellow, or a milky murky yellow color, or a murky muddy dark color like dark green almost brown,light green-yellow?
what color is it now after you added SMB?
did it ever go clear like water, or go brown when you added SMB?
Did you see a red fume when SMB was added, or did you smell rotten eggs?

what color are the powders that are precipitating, black, or black and white or gray?

Two reason's the stannous test may not show up even if gold is in solution.

oxidizer like nitric acid still in solution re-oxidizing gold back into solution, this free nitric would also keep the SMB from reducing the gold as the nitric would just keep redissolving it.
Or
If you had sulfamic acid you could add some and give it a good heating, or if you have some gold you could add it to solution heat it strongly and concentrate it some,to use up any free HNO3,to see if this was the problem, and see if solution would precipitate the gold when cooled

another reason stannous will not test for gold in solution is if the gold is already reduced, such as when it does with tin in solution making colloidal gold, here filtering should give you an idea if tin is in solution, it will be hard to filter going very slow if tin is involved.
If the solution was very hard to filter I would suspect tin colloids and we would have to work hardto get gold back from them, lets hope that is not the case here.

The solution looks dark and dirty, like maybe you did not get all of the copper out of the gold then dissolve it up with the gold, gold can also be held some-what in solution with a dirty solution the copper could also be trying to reduce and the gold plating to it, and both of these held or holding each other in solution, (tin, excess HNO3, or nitrate salts,and or too much SMB, could complicate the situation, everything swapping those electrons around nothing gets settled, everything having too much fun playing ball with those electrons keeping all them little metal cations and anion ions and atoms excited trying to get the ball)
Especially if oils or other contaminates may be involved, a strong heat and concentrating the acid may help.
What is funny, to me the solution looks like your Q-tip purple to me, or about the same color, but then again I cannot tell for sure what color it is,are you sure you had karat gold and nothing else in this mix?
sorry about that I seem to have more questions than answers, the solution does not look anything like what I expect to see from refining karat gold.

When working with karat gold you really should use good chemicals (not home made nitric acid unless it has been distilled), The gold should also be tested to be sure you do have karat gold and are not mixing in plated scrap by mistake, your silver should also be tested.

if solution filters easily and suggestions above do not help then add a copper buss bar and some heat, and cement out the gold.

When you get the gold back I would save it for now, and wait until you had a little more study before trying to put it back into solution,depending on what you find out while getting this gold back now, can make a lot of difference On how I would treat it from here on.
 
My thoughts exactly it looks exposed to bright light "sun" and mixed, " digested " my take on this would be to evaporate , wash organics out " if any " evaporate, and use dilute nitric, for
a removal of copper n silver. canter, wash suspended, dry, n second nitric, for purifying, , for a 98 plus melt, look for 8 to 10 grams of AU, i have dirtied a lot like this myself,
good luck with this, your not in a loss position, your still in the pre reduction stage. Cheers, well said butcher , i think you have given no1special the skinny on this
 
if you happen to be wondering how you can make silver chloride when using poor man's nitric, its because of the salt left in the solution. you have to freeze the solution to remove the salt and still cant get it all. some recommend adding silver nitrate to the solution (creating silver chloride) to remove the last bit of salt. to me, thats a very round about way of doing something.
 
Ok getting ready to hit it again. To answer a few of butchers questions. There is a good chance that got contaminated as I had added some previously dropped powder and a couple cell phone boards that were scraped of all components with a knife (I wont mix again. As for colors the solution was a light green color before smb which turned to a dark browninsh green when smb was added. Some brown powder did settle and covered the bottom of the jar, which i have decanted and washed with hcl boiled for a couple mins decanted off acid and water washed so far... will get back to you on the weight when done washing and get it dried out. The color now is a clear brownish tint not unlike a glass of tea. Will try to filter some and see how that goes and turn the heat on it again and be back with my findings
 
Well it seems that things were not so bad. The powder that had already fallen ended up amounting to a 6g pellet, and when i tested the solution that i had inquarted with and dropped out silver with salt, it tested pos on stannous and i heated it and added smb and wall-ahhh the rest of my powder is settleing as it type and it looks to be close to amount that i had before. Thanks to butcher and all those who guided me through the process. When it all gets done I will post a pic of my pellet.
 
Am from Poplar Bluff. Well here is how it went today. First I boiled down the dark solution and when it started getting thick, salt formed confirming that was nitrate salt in there no doubt. The powder that had fell already was more than i thought however and produced 6gs of pellets. Any how after filtering out salts I put the solution back on heat and the color changed to a light lime green and once again tested pos with stannous. Meanwhile after filtering the silver cloride off the inquarting solution which was a light blue color changed to a light green after filtering, also tested pos again. I added a pinch of smb and the color went to a dirty dark brownish green again and started dropping a brown powder so i put on heat. After it warmed up the powder dissolved again and then the solution turned to a glorious clear yellow. Once again there was still nitric in there was my conclusion so i kept on heat and evaporated down for a while then added one of my pellets and saw no reaction. I then doubled volume with water which had no affect on the clear golden tinted color and when i added a spoon of smb and stirred it turned first clear then darkened gradually and soon started dropping that wonderful brown powder and i left to settle over night. As for the origional solution it once again started forming salt when it was reduced to syrup, and last thing i did was remove from heat and added more hcl which turned it back to a light lime green which i plan to filter off again in morning and add heat to see what it will do, It still had a pos stannous reading last time i checked. Thanks for the helpful advise and here is a pic of my pellets from this so far.
 
Are you talking about a radio tower? My career has been working on up to 800 ft smoke stacks and radio towers are about the only structures around here that tall... by the way i would have been 4 then.
 
So what did u do just build like an erector set piece by piece? I have been on steel smoke stacks before and while all stacks are designed to sway with the wind, the 250 footer with a 12 foot diameter that I demolished at a US steel plant in Pittsburgh PA was rocking like nothing else i have ever been on. Took a few mins to quit swaying after we climbed down and was on the ground.
 
We would stack it 20 foot at a time, would stand up a 20 foot section, we had a double drum winch with a V8 engine and transmission, me and another guy would climb the twenty foot section with a pulley and the 1/4" winch line, hang the block, there is another block at the base of the tower for the 1/4" line, end of this line goes to a GIN pole a 24' long six inch pipe with a rooster head (block that swivels around with the 3/8" cable), the winch operator would raise the gin pole, with the 1/4" line, a tag man on a rope pulled the gin p[ole away form the tower as it is raised, we would mount the gin pole to the tower, in set on a hook plate at the bottom and we used a sort cable with a turn buckle to lash the pole at the top of the tower section.

now this gin pole stuck up 14' taller than the tower section, from the winch a 3/8 cable ran to the tower bottom through an 8" pulley up the tower through the gin pole pipe around the swivel rooster head pulley in the top of the gin pole and back to the ground to a 150 pound weight made out of pipe filled with lead, rings welded on each end and a sling with two clevises, this weight was tied a little more than half way up this twenty foot tower section, the cable was clevis-ed to the top of that section, the tag man had his rope tied to the weight, and looped around the bottom leg of the section, the winch operator would raise the section to us using the 3/8" cable winch drum, the tag man kept it pulled away from the tower, when the top of this section got to us tower men we undid the top clevis, wave our arm to the winch man to raise the section, the weight and mid of this section moved up to the rooster head, and the bottom of this section would clear the top of the tower, we would wave our arm to signal the winch operator to stop, the we would swing the section around , using spud wrenches we would line up the bolt holes, signal the winch operator to let the section down, he would stop when he felt he weight off of the winch, we would bolt the tower section to the tower, now we were a 40' tower.

we I would climb to the top carrying the block and 1/4" line up and hang it on top, climb back down to the rooster head and straddled it the other tower man would undo the gin pole at the center and straddled the gin pole, then we would wave our arm up, and the winch operator would raise the gin pole up between our legs, now that the rooster head was 14 foot taller than the tower we sit the bottom of the gin pole hook on a step of the tower and strapped the gin pole to the tower, and climbed into position for the winch operator to raise another section to us (the ground man was preparing the section as we moved the gin pole, after raising and bolting the section on we again raised the gin pole while the tag man prepared to send up three guyed wires, we mounted the guyed wires, and came down and anchored the guide wires pulling them tight with chain comealongs the tower was sighted with surveyors scope, from two angles the straighten it as we tightened once tight to specs and the tower straight we clamped off the guy wires, got back on the tower and stack another 60 foot and guy wired, after 500 foot we would hang the beacon and side lights, mount antennas, spot paint the tower, pack up our equipment, go to the bar, then we were on the road to the next job site to stack another tower, hang antennas, to repair a TV tower or whatever,
The tallest tower I worked on was a 16,000 foot tower.

The tower has to sway, if it didn't it would break and come crashing down.

It is one of those jobs you just love never a dull moment.
 
16.000 foot tower... that's impressive, especially as the tallest man made object is Burj Khalifa at 2722 feet. :mrgreen:
It was really interesting to hear your stories about the mast work, thanks for telling it.

Last week I was involved in a 300 ft (99m) wind measuring mast. All the mounting and climbing was done by four other guys and the lifting of the sections were done by helicopter. The mast were assembled in just one day but the sensors took more than two days to mount. My part was to design and mount the data acquisition system and calibrate it all, I only had to climb to 8 m to mount the radio antennae for the computer.
This was my first mast and it was really interesting to see how it was made... and a bit dramatic when one of the connection boxes got tangled in the guy line at the top and fell from 90m height. Luckily it got two cables over the guy line and slide along the wire down to the ground... just the wire we were standing under. To run along the plowed road was a bit stupid so after a few meters I turned and threw myself straight out into the deep snow in the forest and the box came sailing by me at 20 m height with the cables trailing. We managed to catch it by the cables before it hit the ground, so in the end I just needed to cut off a short bit of the damaged cables and glue everything that was yanked loose inside the box. The next day it went up to 98m and everything worked just fine. 8)

Göran
 

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