# no reaction when I added SMB



## ctgresale (May 16, 2013)

Ok need a little help with what went wrong. Did a small batch of fingers with HCL/proxicide (pic#1). 3- HCL washes afterwards, added bleach and dissolved the foils then added distilled water to make 3 times the volume (picture #2). Then I just let it set for 2 days, did not heat. Then mixed up Sodium Metabisulfite in some regular tap water and when I added it to the AuCL3 I got the immediate color change from bright yellow to clear ( picture # 3), but it never changed past clear, no brown precipitation at all, just stayed clear with a slight blue tint to it. Also not sure now if I added too much SMB because when I added it when it was mixed in the water and it did not start the reaction I added more just as the power. Still the same color though. When I added SMB the 1st time I did get a small sulfur odor.


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## kkmonte (May 16, 2013)

Hmm, how much in foils did you dissolve? Or how much raw materials and what were they? (Assuming fingers) ? It looks good and clean, but since you got the color change, are you sure you don't see any brown powder on the bottom? Why is it in two containers on the last picture?

Also do you have stannous chloride to test your final solution to see if there is any dissolved gold left?

Ken


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## Claudie (May 16, 2013)

Tap water has Chlorine in it, that could be part of the problem.


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## ctgresale (May 16, 2013)

definitely no solids in the liquid at all, not even SMB. There is 2 containers because once I added the dissolved SMB and tap water it was getting near the top so just as a precaution I poured off into 2 containers. Did not check with stannous chloride, LazerSteve had just sent me some but had not made any up yet. There was between 2 and 3 lbs of fingers, and I haven't done anything to get any gold out yet. Added SMB to the yellow AgCL in pic # 2 and went straight to pic # 3. Nothing has come out of the solution since the start.


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## Claudie (May 16, 2013)

How much water did you use to mix the SMB? It appears to me that you have a lot of extra water in there and being Chlorinated water, could be stopping the Gold from dropping. 
Is your SMB old?
Is that your kitchen range that you are working on?


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## ctgresale (May 16, 2013)

water originally was 2.5 cups, more now since I keep adding when there was no reaction. Not working inside on my stove, just used white for the background when I took the picture. When I say there is no solids in there I mean it's crystal clear, no powder, no gold, no undissolved SMB, nothing. I'm starting to think it is too much CL left in solution. What is the best way to handle that ?


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## ctgresale (May 16, 2013)

SMB was couple months old, bought it off ebay from a winemaking supply house


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## kkmonte (May 16, 2013)

Nah I wouldn't say so, because if there was, then your solution would still be yellow. When you dissolved the foils by adding bleach, did you strain it afterwards? are you sure all the foils were dissolved? 

If there is too much chlorine in the solution, then when you add the SMB, nothing will happen (at least in my experience), no color change, no nothing. To get rid of the excess chlorine, you could try heating it (don't bring it to a boil, cover with a watch glass, or if its in a coffee pot, it might have a built in cover). By heating it you will drive off the excess chlorine.

I've had too much chlorine, and like I said, added the SMB and the solution still stays yellow, and sometimes you see the SMB powder in the solution (i've never dissolved it in water first, i usually just add the powder directly to the auric chloride). 

I don't think it's the tap water, Laser Steve always says he uses tap water (far as I can recall).

So wow, 2-3 pounds of fingers worth of flakes, depending on the quality of the fingers, i'd estimate 3.3-5.5 grams of gold. How much SMB did you dissolve in how much water? I hope it was at least 5-6 grams worth of SMB.

I'd say make your stannous, by not having any (as butcher always says) you are working blind. A simple test with stannous will tell if you dissolved gold is still in the solution (doubtful since its not yellow anymore), however it's tough to say where it went!


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## bee (May 16, 2013)

seems tap water isnt a problem ,
as only used to make SMB solution.
look at your last pictures the water is not clear 
kkmonte is right the yielding should be around 3grams. but where is gold gone?
put on low heat for 1 to 2 hours i donot think there is excess chlorine as 2 days are enough to drive off any excess chlorine but assume there is really a great volume of bleach but then again solution shouldn't change color.
now what i am thinking is when you dissolves the foils you use little bleach and may be you didnot stir your solution when you add the bleach did you stir and is there any white powder precipitate(it should be precipitate as this is NACL and when gold is dissolve its precipitate out.) try to redissolve the left over residue .
and if there is no residue then the gold is still into water.
we find two possible ways either the gold is into left over residue.(which is 90% not possible)
or there is great volume of CL then you need to heat it below boiling point for 1 to 2 hours if there is any gold it should be precipitate within 2 hours.
carefully recall all your steps and try to solve this puzzle and remember the gold is into two possible places which i mentioned above.
thanks
bee


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## ctgresale (May 16, 2013)

I'm going to try and find a couple more pic, and I have a video of the SMB pour in the AuCL with the color change


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## butcher (May 17, 2013)

NaClO sodium hypochlorite, what we call bleach is a basic substance, the NaOH sodium hydroxide in solution helps to keep the chlorine gas dissolved in this alkaline water, the bleach can be about 94% water.


HCl Hydrogen chloride is a gas, when dissolved in water it makes an acid we call hydrochloric acid or HCl acid, this acid is about 68% water

If we mix this acid with a base we make a salt and neutralize both the acid and alkaline solution around pH 7 if in correct proportions,

HCl + NaOH --> NaCl + H2O
Here we took a strong acid and a strong base both can be dangerous to your skin, and mixed them into a solution you can eat or wash your eyes out with.

(Caution unless you know what your doing do not try this}
trying to do chemistry without studying and understanding completely what your doing, not only can it make a mess but it could blind or poison you.

When we mix the NaClO with acid we generate chlorine gas this is what oxidizes our gold, we also try to do this with an excess of acid, the acid is reduced by the oxidized gold to form chlorides the gold and three chloride join to form a salt of gold chloride AuCl3.

What happens if we have limited acid over use Hypochlorite to make chlorine in solution to dissolve our gold, the acid is turned to salt and the solution can become basic or even alkaline which can hold excess chlorine gas in this salt solution easier, than an acid solution will.

Cold solutions hold most gases like chlorine in them easier than a hot solution.
Chlorine will stay in an alkaline solution longer than it will a neutral solution, and is driven off faster in an acidic solution.

We could go on with what happens when we dissolve gold but you can read more about that on the forum, here is one place to read a little bit more kind of related.

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=37&t=16434&start=20

I do not know you have gold in solution, as far as you know you do not either, you may believe you do because you seen it disappear when you put it into acid and added the sodium hypochlorite, but without testing you could no longer see it, so your gold just disappeared, here is where using your test solution will prove to you where your gold is, by allowing you to see a reaction of reduced gold in your stannous chloride test, the violet color verifies your gold is or is not in solution, it is you eyes to allow you to see the gold when you can no longer see it. Note the stannous chloride test must be able to reduce the gold for the test to work, if you have too much oxidizer in solution like chlorine the gold will not reduce so you have to remove the oxidizer before the test will work.

This is also true for precipitating your gold with sodium metabisulfite, the SMB will not be able to reduce the gold in solution back to a metal if you have too much oxidizer like chlorine in solution, which just keeps re-oxidizing the gold back into solution as ions.

What could have happened with your gold? Is it still there?

What may have happened is you used way too much bleach, put your gold into solution, but also raised the pH of the acid to salt water or a basic solution, which will hold chlorine, besides the water involved in both the acid used, and the bleach used, water is also formed in the reaction, so at that point you could have had a pretty dilute solution of salt NaCl gold salt AuCl3 and water, mixed with chlorine.

Then you added sodium metabisulfite and added more water to the mix, which will also form bisulfate salts as the SO2 gas leaves solution, the chlorine overwhelming your SMB keeping your gold in solution.

With just a little gold salt dissolved in solution the color is yellow, but with as much water as you have and all of the other salts in solution and as dilute as it is, you may have dispersed the gold in solution so much it diluted the yellow to where you cannot see it.

Heating this solution will concentrate it and all of the different salts involved, it can also help to drive off free chlorine gas (better if solution is acidic), the SMB has already reacted and may or may not reduce your gold when you concentrate the solution, it could just form a more concentrated bisulfate salt, along with the other salts in your solution.

I would concentrate the solution, to drive off chlorine, when it gets concentrated, you could see salts forming, or maybe even some gold powder, if you used way too much SMB, maybe even elemental sulfur powders could form, these salts if formed depending on conditions could be base metal chlorides, and or sulfates, NaCl, and even chlorate, if too much bleach, many of which would be water soluble.

I would not concentrate it too far, I would bring it down in volume to not less than half the volume that it was when you dissolved it.

Check pH and add acid if needed, after it is more concentrated, to keep it at least slightly acidic.

If you wish to check to see if chlorine gas is coming off the fumes when heated, put a few drops of ammonia in the lid of the ammonia bottle the ammonia will fume hold the cap in the fumes coming from your solution while evaporating, when the chlorine and ammonia fumes mix the light colored smokes, will mix, and gets whiter forming ammonium chloride gas the white visible fume coming from the cap of ammonia proves chlorine gas, do not get the ammonia into your solution.

Do your stannous chloride test, if positive you found your gold,you can now see where gold is, you also know the chlorine is low enough to be able to reduce the gold.

At this point if gold is in solution, adding more SMB could precipitate your gold, or it may not, depending on conditions, you may find your only alternative if gold is in solution and will not precipitate is to cement the gold out of the acidic solution with a large piece of clean metal copper.

Remember your testing solution is your eyes to see where gold is and where it is not.

Now I cannot say that what I described above is, what has, or will happen, just what I suspect.


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## ctgresale (May 17, 2013)

Thanks guys, let me do this step by step again add some numbers to help.OK after removing the foils from the fingers, I filtered 3 times with fresh Crown Muriatic acid 31.45% (pH < 1). pic #1 is a cup of fresh HCL and the foils. Then in added the HomeDepot outdoor bleach (MSDS-4.5-5.5% sodium Hypochlorite, <1% Sodium Hydroxide w/pH 12.5-13.5) Got the strong reaction as all the foils dissolved where there was only some green solder mask left. Filtered that into another container and diluted it 3 times volume with distilled water, which is pic #2. Then it sat for 2 days. I dissolved the 20g+ SMB in tap water in 2.5 cup measuring cup and added to the yellow in #2. It changed from bright yellow to clear immediately but never darkened, still today ( 24hr since adding SMB) is the same color as pic # 3. Butcher I just went and checked the pH level and it is 6.4 .


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## butcher (May 17, 2013)

So if I understand this,

You had about 3 grams of gold, which could possibly be dissolve in around 15 ml HCl. 

You used a cup of HCl, which is enough HCl acid acid for about 2 troy ounces of gold.

Then you you do not state how many milliliters of bleach was added, but you must have added quite a large amount of sodium hypochlorite to bring the pH so close to neutral of pH 6.4 now, and then diluted the chlorine in solution.

Let it sit which may not have driven off much chlorine gas, at this pH and temperature, in the dilute solution.

And added 20g Na2S2O5, enough SMB to precipitate about 20grams of gold from solution.

Sounds like you have an excess of everything but gold at this point.


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## g_axelsson (May 18, 2013)

isn't there a need of an acidic solution for the SMB to work? Or at least work efficiently.

I had a solution that didn't drop any gold, but with a couple of percent HCl added all my gold precipitated from the solution. I had a beaker with gold chloride that had dried out totally and I only added water before trying to drop the gold.

But before trying something like this, get your stannous testing kit and start testing! Without it you are totally blind and you might throw your gold away by mistake while trying to get gold out of something that doesn't have gold in it.

Göran


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## butcher (May 18, 2013)

Goran that is what I also believe, the water and the acid is what we need to precipitate gold for the reaction of SMB to take place.


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## ctgresale (May 25, 2013)

OK Guys, I'm back, and he is where I'm at. First I have had it on heat to remove as much dissolved bleach in solution that I can. Also continuing to leave on heat to remove a little over 1/2 of the volume that I previously had. It was starting to get too dark so cut it off for the night, but I believe there is right about 2L of liquid left. Went ahead and made up a fresh batch of Stannous Chloride made up from Lazersteve's recipe and will try and get some more data some. The liquid is back to a bright yellow with a slight brown tint to it, and PH is lower than 6.0 because that was the lowest reading in had on my chart. I think is that I can see a few small gold flakes floating around in the solution. so we'll find out if we've been able to save the project. Thanks in advance for everyones help and comments, and look forward to more once I get some picture posted to shed more light on how things look.

Thanks
Steve


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## Alentia (May 25, 2013)

Your gold did precipitate and your solution was perfect. It is just the amount of gold you had there was so little, so that you think solution is clear. You should have waited for at least 12 hour and would found tiny brown layer at the bottom. Swirling it about 1 hours after SMB would bring some of the gold at the middle.


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## ctgresale (May 25, 2013)

Alentia- just so you know, I did wait, it's been over a week, nothing ever came out.

Here is the updated pictures- Pic A- 1300mL solution from both coffee pots heated below a boil for 24hrs, reduced liquid volume by 1/2. Pic B is the Stannous Chloride test with fresh solution from the new 1300mL solution. Again this was harvested from gold fingers only, and no this is not a grill that is or will ever have food on it- only used for scrap/incinerating, etc. Look forward to your comments. 


View attachment 2


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## butcher (May 25, 2013)

That looks like about 8 cups of liquid, the orange color could be gold in solution, but with that much solution, It is a bit puzzling, (for that volume of liquid with that color I would expect much more gold in solution), maybe the SMB added earlier may be effecting the color, to get that concentrated of a look with such little gold for that much solution, so this makes me think the color may be deceiving, also I would expect salts to form if you have diluted the solution down from a much larger volume, I do not know if the solution is still hot in the picture, and salts are still dissolved in solution or if there just are not any forming yet, your stannous chloride test does not show much gold in solution on the Q tip, I am unsure if that is tin powders you put solution onto, but it is showing a little more violet look there.

You will want the solution acidic and diluted before trying to precipitate.

With the amount of fingers processed I would expect somewhere around 6 grams of gold, that amount of gold could go into solution with around 4ml of HCl per gram, which would be around 24ml of HCl, you have at present about 8 cups or 1800ml of solution, even after the evaporation you have done so far, to me this is still way too much solution, and if you haven’t added any HCl acid the pH is probably still to close to being basic.

I think I would keep evaporating it some more (you may see salts form) once you get it down further, if they do you and these salts start to build up too much, you could remove the salts from solution into another clean container, keeping them covered with some water, to keep wet for the time being (and test them later),

I would bring this solution down in volume, way down in volume, acidify with some HCl after getting the volume down much closer to the amount of solution you would expect 6 grams of gold would be in (closer to only a cup or two of solution at most),bringing it down to a lot less volume than you have now, and retest the solution with stannous chloride after the solution is concentrated and it has been acidified with HCl.


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## ctgresale (May 25, 2013)

Thanks for the input butcher. With the stannous test, the qtip did not show up very well so I put another couple of drops on a cotton ball, that what is in the center of that dish. As for the salts, I've been using a crock pot to heat with so there have been some salts form around the top when the lid was on, but not any in solution. I let solution cool for 24hr, ran through 3 coffee filters to get a few gold flakes that formed, and transferred to the fresh container. I'm going to continue on to decrease the volume in half again and retest. I'm not sure what those # are on the side of the coffee pot but when I transferred the solution I used a measuring cup and there was exactly 44oz.


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## butcher (May 26, 2013)

If there are 8 fl oz per cup, 44 fl oz would be about 51/2 cups, or about 1300 ml.

118 ml of HCl will hold an ounce of gold easily, more if concentrated, (This is from Hokes statement, four fluid ounces of HCl and one fluid ounce of HNO3 will dissolve an ounce of gold).

So 4 fluid ounces is about 120 ml or about 1/4 cup so a quarter of cup of HCL will dissolve an ounce of gold (with a strong oxidizer like nitric acid), and this solution can be concentrated down quite a bit (de-Noxing solution), and still hold the gold in solution as chlorides.

With HCl/NaClO (bleach) the volume is tremendously higher, for a couple of reasons (the bleach is almost all water), and the acid is neutralized by the bleach forming salts in solution, so with this solution you would have quite a bit more volume of liquid involved and could not evaporate it down as far before it became just one big lump of salt, with gold chloride salt being one of them involved, but at this point you still have an awful large volume of liquid for having only six grams of gold in solution.

As we discussed above with the HCl and bleach we neutralize the HCl and can make NaCl and other salts in solution, you may see these as you evaporate the solution, with the SMB added we will also have some sodium sulfate or bisulfate salts, all of these are water soluble.

The gold may or may not begin to reduce as you concentrate, (it probably will not as the SMB has already reacted previously), but just in case. you can dissolve the saved salts in water to see if any gold may have also reduced with them (if the gold is reduced to metal, brown or black powder, it will not dissolve with the other water soluble salts).

The cotton looked like powders to me, that makes much more sense now, I believe you are getting close, we can see the violet from your stannous chloride test, not as violet as I would expect for that much gold in solution, so I am guessing we may still have some chlorine to get rid of from solution, (keep in mind also if the solution is not that acidic it will also hold chlorine easier) but it is looking like you are getting closer to getting your gold, I would like to see that stannous reduce the gold to a strong violet colored Q-tip, or cotton ball, (you will probably need more HCl acid after removing more liquid volume), if we can get the gold to reduce well with the stannous test, then we should be able to bring the (acidic) solution back up with water diluting it before trying to precipitate the gold again with fresh SMB.

These are just my ideas of what is going on, and how I may try to deal with it, although my Ideas may not always be right, and there could be other or better ways of going about this to get your gold from solution.


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## birdflu78 (Jun 9, 2013)

I would like to post my experience, maybe it will help or maybe not. I had a batch of hcl/bleach solution and dissolved gold from dinner plates. I had over a liter of solution when I was done. I waited a couple of days to let the chlorine dissipate and added SMB one evening to drop the gold. I put the container away in the shed. The next morning I checked the jar to see how much gold powder dropped. The solution turned clear but there was no gold powder in the jar. I know there was some gold in the solution and that I had added enough SMB to get a reaction. I decided to set the jar outside in the sun to see what would happen. After an hour in the sun all of the gold precipitated and settled to the bottom of the jar. I guess the solution was too cold when I added the SMB?


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## butcher (Jun 9, 2013)

sunlight as well as the heat has a catalytic action on chlorine in water:
2H2O + 2Cl2 --> 4HCl + O2


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## birdflu78 (Jun 20, 2013)

As always thanks for the info butcher. I used to be very good at chemical equations but that was so long ago!


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