Prepping to drop with SMB - SUCCESS!!!!

Ok so last night I finally had time to work on this some more, and successfully put my foils into solution (using HCL + CL (standard unscented Clorox) approximately 2 cups HCL and 3/4 cup Clorox) that I had recovered from fingers, etc with AP in this thread http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=37&t=17416. Positive Stannous test for gold and preparing to dilute and drop the gold out with SMB. (see pic)

Now as for my question, I cannot detect the scent of Chlorine gas but I'm not certain it's all gone yet. It was originally at the 700ml level on the beaker in the pic (-edit- before heating and evaporation I let the reaction work for a good 30 mins or so until Chlorine gas stopped off-gassing) and evaporated it down to just over 600ml (to drive off any remaining Chlorine), let it sit in place to cool down gradually and once cooled it sat at just below 600ml. Is there an easy ph test I can do to check if the Chlorine is fully out of solution before I aggravate myself by attempting the gold drop and having it fail from Chlorine being still present?

I'm not sure if I understand what you've said. I think you're saying you heated it for 30 minutes and reduced the volume by 100 ml. If that is correct, you are probably ready. If you want to be positive, you can just let the solution sit for another 24 hours.

I don't believe a pH test will tell you anything about remaining chlorine. Butcher has mentioned a simple test. Put a tiny bit of household ammonia in the cap from the ammonia bottle and hold it close to your solution. If there is still chlorine coming off the solution you should see the formation of white ammonium chloride fumes. I believe that's correct. You can search butcher's posts to be sure I got that right.

Dave

FrugalRefiner said:

I'm not sure if I understand what you've said. I think you're saying you heated it for 30 minutes and reduced the volume by 100 ml. If that is correct, you are probably ready. If you want to be positive, you can just let the solution sit for another 24 hours.

I don't believe a pH test will tell you anything about remaining chlorine. Butcher has mentioned a simple test. Put a tiny bit of household ammonia in the cap from the ammonia bottle and hold it close to your solution. If there is still chlorine coming off the solution you should see the formation of white ammonium chloride fumes. I believe that's correct. You can search butcher's posts to be sure I got that right.

Dave

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Close. I allowed for 30 minutes of digestion, filtered then heated for about two hours just below boiling which evaporated about 100 ml off and let sit overnight

That would have been my second guess, except I hadn't heard the 2 hours or overnight rest. You should be good to go.

Dave

Here is a test you can use to see if chlorine is still coming off of the solution you are heating.
As you heat your solution you will see vapors, clear white fumes coming off of your solution, these will be gases of water and possible chlorine at first, until the solution is very concentrated then HCl will vaporize off in fumes (but at that concentration you would begin to see salts form, from the hydroxide of your bleach and chlorides of your HCl).

You may be able to smell some chlorine vaporizing with the water, but it can also be hard to tell.
A test for chlorine gas:
Pour a cap-full of ammonium hydroxide in the cap of the household ammonia bottle about half full, the ammonia will fume from the cap, hold this cap in the fumes of the fumes coming off of your heated solution of suspected water fumes or chlorine fumes, if the fume contain water you will see no reaction, but if your heated solution is still vaporizing off chlorine, the ammonia gas and the chlorine gas mix to form a white smoke of ammonium chloride smoke clearly visible reaction.

Take note You do not want to spill the ammonia solution.

Another indication if you have driven off most of the chlorine from your solution is the stannous chloride test, testing your solution before and after, with excess chlorine the SnCl2 test may not indicate gold (violet reaction) even if gold is in solution if you have excess chlorine oxidizer, or it may go violet for a second and them disappear, as the chlorine re-oxidizes the gold which the SnCl2 is trying to reduce, but after you have removed excess chlorine from solution the stannous chloride test will stay Violet indicating the gold can be reduced back to a metal (colloid), by the SnCl2 test solution, also indicating you precipitant like SMB will also be able to reduce the gold back to metal.

FrugalRefiner said:

That would have been my second guess, except I hadn't heard the 2 hours or overnight rest. You should be good to go.

Dave

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Sorry about leaving those details out/in a confusing state.

At any rate, I went ahead and started the drop with SMB (as I don't have any ammonia to attempt the test mentioned) and the results are looking VERY promising :mrgreen:

Wow that's a lot of solution. Looks like the same jar I'm using for my first batch. I processed a little over 800 grams and have about a quarter that amount. Still gassing off chlorine though. Just got home from work about an hour ago so I'm getting a late start tnite. Looking good, Capt. Good luck.

Joe

kane333 said:

Wow that's a lot of solution. Looks like the same jar I'm using for my first batch. I processed a little over 800 grams and have about a quarter that amount. Still gassing off chlorine though. Just got home from work about an hour ago so I'm getting a late start tnite. Looking good, Capt. Good luck.

Joe

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Yeah it's my first refining batch ever so not perfect obviously, I do however make sure to learn from mistakes tho . The solution qty started out about half that amount then I added the filtered diluted HCL I used to get the residue off the coffee pot I used to initially digest it all in, which I then added to what was there currently and then proceeded with the drop.... so yeah qty got a little crazier than I had planned on I'm just glad it's working as well as it is tho.

Captobvious said:

...the results are looking VERY promising :mrgreen:

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WooHoo! You got Yoohoo!

Looks good.

Dave

One question. After ridding the solution of excess chlorine, is it recommended to filter the solution again? Even if no salts have formed after letting it set overnite?

When in doubt, filter it out...
Just remember, the filters may contain some PGMs so run a fresh batch of HCL+bleach through to redigest anything that might be there as well as any other containers used. I filtered into 2 coffee pots and there's visible powder stuck to the sides.
And remember to let it sit. Patience is what needs to be learned first and foremost. It may drop more gold after sitting.
B.S.
Only about 100+ more pieces of glass to disolve untill I can dry and measure my prize...

kane333 said:

One question. After ridding the solution of excess chlorine, is it recommended to filter the solution again? Even if no salts have formed after letting it set overnite?

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No, I wouldn't. If you filtered the solution good after dissolving all the gold, there really shouldn't be anything to filter. If you do want to filter it again, you'll have to really clean out your filter again (spray all the auric chloride out of the filter). I'd probably let it sit again for a bit, one time I had dumped my solution from one beaker to another (1L to 1L) and i think i disturbed some hidden chlorine, because when I went to add the SMB it all fizzled at me.

I'm not certain if this is normal as this is my first refining. When I got home from work tonight after leaving the solution to settle for approximately 28-30 hrs at this point everything looked to have settled nicely at the bottom. Tested for gold remaining in solution, test was negative (clear). I siphoned the liquid down until about halfway, and then decanted down to about the last inch, however I'll have to let it settle a bit more as the powder appears to have mixed around a bit. At any rate when it was down to last inch or so and I could get a good look at the bottom it all looked like brown slime for lack of a better term. Once it settles again and I can decant the rest off I should have a better idea of what I'm looking at but everything I've seen before in vids/pics has been a crumbly powder, even when in final solution. Would my situation be just indicative of a small quantity of powder? Also assuming I cannot get it completely decanted off, would it then be best to heat and evaporate off any remaining liquid and allow to air dry the powder?

Once I do the next decanting I'll post some pics as it's rather difficult to see beyond the murk at this point.

At this point I will normally wash it into a small clean vessel using the spray bottle, (small canning jar of 50ml beaker), where it sits on a small electric coffee mug warmer, I can begin the washing procedure, the first washes may need to be done without heat, and giving time for the powders to settle if the gold is fine and still dirty, as the gold gets cleaner it will settle faster and easier, even with heat, the hot water washes can dissolve any lead chloride which can then be decanted while hot, using a suction tool and pipette to remove liquids, so as not to disturb the settled powders , I will normally do the washing procedure, then refine the gold again. the cleaner you get that gold the easier it will clump and settle.

butcher said:

At this point I will normally wash it into a small clean vessel using the spray bottle, (small canning jar of 50ml beaker), where it sits on a small electric coffee mug warmer, I can begin the washing procedure, the first washes may need to be done without heat, and giving time for the powders to settle if the gold is fine and still dirty, as the gold gets cleaner it will settle faster and easier, even with heat, the hot water washes can dissolve any lead chloride which can then be decanted while hot, using a suction tool and pipette to remove liquids, so as not to disturb the settled powders , I will normally do the washing procedure, then refine the gold again. the cleaner you get that gold the easier it will clump and settle.

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I went to bed before I saw your post Butcher, but due to the particle sizes being so small it ended up being more frustrating than anything else to try and decant it, and when I went to evaporate, the powders were getting burped up on the side of the glass or drying to the bottom of my beaker (too hot maybe?) I had transferred to after siphoning/decanting.... sooooo I got tired of that and just decided to filter the powders out and let dry. The filter was still slightly damp so this isn't a final weight, and I'll also be setting it aside for a 2nd refining but will probably wait on that until I have another first refine of my next batch of fingers. What you say makes a lot of sense with as dirty as I'm sure the powder still is (I'm a perfectionist what can I say lol) as it took me 5 coffee filters to catch it all they were so fine, but alas..... SUCCESS!!!

Dry weight of the filters was 6.3 grams, for a final damp weight of 5.4 grams of powder :mrgreen: :mrgreen: :mrgreen: :mrgreen: :mrgreen: :mrgreen:

I finally figured out my new scale and that when I weighed it this morning, I had 3 too many filters in my clean-dry filter weight.

That said final dry weight first refining 2.7 grams

Now that I'm more familiar with the process and the weather is FINALLY starting to warm up (2nd Winter was getting a little old) I can dig into the bucket of memory sticks I've been collecting since I started this batch back in February but could never seem to find the time or weather above freezing consistently to finish. Now to perfect the process on this bucket of poor unwitting memory and video cards! MWahahahaaha!!! (Sorry as an IT guy it's kind of cathartic to destroy these technological creations after a long day of keeping them working! lol)

I'm definitely going to document my next attempt much more meticulously for you guys in the future so, sorry about that. Big thanks to all on this forum that have helped get me this far!

I do not use filters to catch (trap) my gold.

I like leaving my gold in a vessel as much as I can, many times once my gold goes into a ceramic casserole dish the gold stays there almost throughout the whole process, liquids that dissolve other metals are removed but not the gold, I like moving my solutions with suction tools, if solutions need filtering they are transferred to a filter, if solutions need settling before solution is filtered the solutions are transferred to settling jars, heating cooling and settling can also be done in the casserole dish, the gold chloride is removed from the dish last.

Usually after removing oxidizers, and allowing insoluble to settle out the gold chloride is transferred with the suction tools to a clean settling vessel where it is diluted and allowed to settle the silver or lead chloride out of solution, then it is decanted again with the suction tools to the clean precipitation vessel.

After gold is precipitated and solution tested with stannous chloride to insure all gold is out of solution, the liquid is removed from the well-settled gold powder with suction tools.

I will then wash the gold into a small beaker 50ml using a wash spray bottle to wash the gold from the precipitation vessel into the small beaker, this is my gold washing beaker, here the gold is washed sitting on a small coffee mug warmer, when I need heat it is on when I need cooling it is off, I can heat a wash for many hours or let powders settle as long as they need to between washes, the gold is not removed from this small washing vessel only the solutions are using the suction tools, when ready the gold is re-dissolved for a second refining, or dried and formed into small balls ready for melting, the less you disturb gold powders or transfer it from one container to another the better I think it is.

Very seldom do I pour to decant a solution, I will normally use tools to move liquids.

With the suction tools you can remove the liquids without disturbing the gold powders, or other settle insolubles, with the bulb suction you can remove the bulk of the liquid, and then with the pipette you can get down to the last drops, with the bulb suction tool it is easy to move a gallon of liquid, the tool is also handy to start a ciphering hose when transferring larger volumes of liquid like from a five gallon buckets.

A pipette can also be cut and stuck on to the end of the larger suction bulb tool, with this you can get small amounts of liquids deep down in a jar, or remove that last 1/2 inch of liquid from the top of your powders, the smaller nozzle of the pipette on the bulb when you get close to the powders makes it easier to pick up liquid and not the powder, the larger bulb helps you pick up more liquid than you can with the pipette bulb.

When I got a large amount of fine gold that almost never settled (dropped from a dirty solution) I just redissolved it and dropped it again in the same beaker. It came down so much easier the second time and it only took about one hour, time easily saved from the later stage of washing.

Another thing I saw in this thread and a couple of other threads is ammonia used as reagent of chloride gas... does that work? Isn't ammonium chloride made by the reaction between ammonia and HCl gas, not ammonia and Cl₂ gas?

Göran

g_axelsson said:

When I got a large amount of fine gold that almost never settled (dropped from a dirty solution) I just redissolved it and dropped it again in the same beaker. It came down so much easier the second time and it only took about one hour, time easily saved from the later stage of washing.

Another thing I saw in this thread and a couple of other threads is ammonia used as reagent of chloride gas... does that work? Isn't ammonium chloride made by the reaction between ammonia and HCl gas, not ammonia and Cl₂ gas?

Göran

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My understanding of the ammonia test was that it was definitely NOT to be introduced to the solution, only that the solutions vapors be allowed to pass by the cap-full of ammonia, to see if there's a vapor reaction.

Butcher, thanks for the info and advice, I'll most definitely be incorporating these ideas on my next refining

Chlorine gas Cl2 and Ammonia gas NH3 will make a white cloud of solid ammonium chloride NH4Cl and Nitrogen gas.
8NH3 (g) + 3Cl2 (g) --> 6NH4Cl (s) + N2 (g)
(I am not positive, but suspect there may be other reactions like chloramines formed, but it will make the visible white cloud of ammonium chloride to give us an indicator of free chlorine in our fumes).

Hydrochloric gas HCl and ammonia gas NH3 will also form this solid white cloud of ammonium chloride NH4Cl.
NH3 + HCl --> NH4Cl

Here the gas has to contain HCl this means our solution would have to be concentrated or very close to the azeotrope of HCl acid to form HCl fumes, normally our solution is much more dilute as if we concentrated it to the point of gassing off HCl we would form salts, when we are testing for chlorine gas the HCl fumes will not normally be present in the fumes of our more dilute solutions of gold chloride solutions, but if we have free chlorine and we heat to fumes this test will show the white cloud.

Still not sure if this works? Try a few test tube experiments, sometimes this gives us an easy way to get acquainted, we can use Hokes teachings to get aquianted, with other reactions, taking her teaching examples in other reactions you may wish to understand on a smaller scale.