SOLVED -I Need Help With Black Powder After Washing It Clean

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Anonymous

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Hello members,

I have been running my sulfuric cell for my gold recovery and it has been without any problems at all. However, I'm stuck at a certain point and I need some advise.

No# 1. Since this batch is only 8 grams of black powder, how much hydrochloric acid am I supposed to use? By the way, I simply used 70 ml of it and it completely covered the black powder that is still in a pyrex dish. I started to transfer the powder first, but I noticed that after the incineration I did on the filter and powder last night, alot of residue was stuck to the dish, so I decided to just add the acid to the dish, instead of the transfer first.

No# 2. How long does the acid need to sit in the dish before I can transfer it? I noticed that the dish was still letting off steam/fume/gases after I added the solution approximately an hour ago.

No# 3. Once the solution cools down, do I transfer it to a beaker, then decant the acid out, then add more acid, then add heat to it? Once I add heat to it, how long must I keep the heat going?

I've been rereading this thread here, the 2nd post on page 5. I'm now at step 12:
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=52&t=7093&start=80

Other than the above questions, everything is going well, without any problems at all. Hopefully, I won't have any more questions and I can then just pop up a gold button in the "Gallery", but I'm sure I may need to ask more questions to make sure I'm doing everything correct, plus I want to be able to say that I refined e-scrap and made a gold button.


Kevin
 
How much acid really depends on if you are dissolving gold with aqua regia or the hydrochloric acid and bleach method.

Hoke's book say's it takes approximately 4 fl. oz. HCl and 1 fl.oz. HNO3 to dissolve a troy ounce of gold.
Or 118.29 ml HCl and 29.57 ml HNO3 to dissolve a troy ounce of gold
This amount of acids divided by 31.103g/t.oz gives us:
3.8 ml HCl and 0.95 ml HNO3 to dissolve a gram of gold.
So if you have 8 grams of gold you would need about:
30.4 ml HCL and 7.6 ml HNO3 to dissolve 8g of gold, measure out Hno3 and add it in small amounts as needed until gold is dissolved (using heat) so you can use up nitric, without having excess in solution with done, you may find you can get by with less nitric than the calculated amount.

If using HCl/bleach to dissolve the gold, you will need a little more HCl per gram than this as the bleach will neutralize some of the acid.

The HCl/ bleach method is easier if you are not used to dealing with aqua regia.
 
butcher said:
How much acid really depends on if you are dissolving gold with aqua regia or the hydrochloric acid and bleach method.

Hoke's book say's it takes approximately 4 fl. oz. HCl and 1 fl.oz. HNO3 to dissolve a troy ounce of gold.
Or 118.29 ml HCl and 29.57 ml HNO3 to dissolve a troy ounce of gold
This amount of acids divided by 31.103g/t.oz gives us:
3.8 ml HCl and 0.95 ml HNO3 to dissolve a gram of gold.
So if you have 8 grams of gold you would need about:
30.4 ml HCL and 7.6 ml HNO3 to dissolve 8g of gold, measure out Hno3 and add it in small amounts as needed until gold is dissolved (using heat) so you can use up nitric, without having excess in solution with done, you may find you can get by with less nitric than the calculated amount.

If using HCl/bleach to dissolve the gold, you will need a little more HCl per gram than this as the bleach will neutralize some of the acid.

The HCl/ bleach method is easier if you are not used to dealing with aqua regia.
Thanks, that gave me a better understanding, which raises another question.

Do I need to add bleach to the HCL? I never added any at all. And do I do the same thing once I transfer to the beaker and decant and filter the solution?

Kevin
 
Kevin, if you add some bleach you will dissolve the black powder and then just proceed with the steps of precipitaing your gold with SMB.
Take care!
Phil
 
philddreamer said:
Kevin, if you add some bleach you will dissolve the black powder and then just proceed with the steps of precipitaing your gold with SMB.
Take care!
Phil
Got it!... Thanks Phil.

Kevin
 
Am I not doing something right?

I added bleach to the hydrochloric acid, which my black powder has been in since last night. I added heat to it, but it doesn't seem to dissolve the black powder?

How long, on average, should the HCL-CL take to dissolve the powder I have, which is approximately 8 grams? So far, it's been approximately 15 minutes the powder has been on low heat.

Kevin
 
testerman said:
Am I not doing something right?

I added bleach to the hydrochloric acid, which my black powder has been in since last night. I added heat to it, but it doesn't seem to dissolve the black powder?

How long, on average, should the HCL-CL take to dissolve the powder I have, which is approximately 8 grams? So far, it's been approximately 15 minutes the powder has been on low heat.

Kevin

You don't heat your solution when adding bleach to the HCL. This goes against trying to keep chlorine in solution for converting your gold powder to gold chloride. If you heat the solution, it will drive the chlorine out before it's had the chance to do the conversion.

Your solution should be room temperature or cooler. Add small increments of bleach and stir well.... give it time. Maybe an hour before adding a bit more.

Keep in mind, there may not be much gold even though it looks like there is. Black in your solution could also be dirt & trash.
 
Palladium said:
Is that a pyroceram dish or does it just say pyrex?
My internet is down right now. I'm using my phone.

This is the dish I'm using. I have Pyrex dishes, but I don't think this dish is.

Sorry, but I don't know how to resize pictures on this phone.

IMG_20130129_123238.jpg

[UPDATE]
Internet back up, plus I added the word in red above.
 
Kevin,

STOP!! Do NOT heat that dish on that burner the way you have it in your photo!

1. That dish is not rated for stove top use, which is what you are doing using it directly on the heating element.

2. The coil type burners are not the best choice for heating any type of dish, including stove top safe types, because they create hot spots on the coils and leave cool spots in between. This can easily lead to thermal shock induced failure of your dish.

3. Always put your primary vessel inside a secondary containment vessel so if your reaction vessel fails your acid and values are not lost into your hot plate.

Others will probably add further advice but I want to stop you as fast as I can.

Dave
 
Best $35 you will ever spend. You can heat these any way you want to. I have even used a blow torch on these things.
http://www.ebay.com/itm/Lot-of-5-Corning-Ware-Blue-Cornflower-Bake-Dishes-PYROCERAM-Modern-made-USA-/200886377657?pt=LH_DefaultDomain_0&hash=item2ec5c2dcb9
 
FrugalRefiner said:
Kevin,

STOP!! Do NOT heat that dish on that burner the way you have it in your photo!

1. That dish is not rated for stove top use, which is what you are doing using it directly on the heating element.

2. The coil type burners are not the best choice for heating any type of dish, including stove top safe types, because they create hot spots on the coils and leave cool spots in between. This can easily lead to thermal shock induced failure of your dish.

3. Always put your primary vessel inside a secondary containment vessel so if your reaction vessel fails your acid and values are not lost into your hot plate.

Others will probably add further advice but I want to stop you as fast as I can.

Dave
Thanks for the advise Dave, yet, at the time I uploaded that photo, I had already turned it off.

The dish IS a Pyrex. I confirmed it after checking on the powder.

I do have a more dishes I can put that in. I have been looking for one of the hot plates that's solid all the way around. I do like them better too, and I've seen more people using them than the kind I'm using. I'll upgrade soon. I'm also going to transfer everything in my beaker, then put the beaker in that dish (with some water added) to make sure that if the beaker breaks, it'll be contained in the pyrex dish.

What comes to mind is that there are different methods of doing this, and from the Tutorial I've been reading, I should be using Nitric Acid along with the HCL to dissolve the powder, yet, others use bleach with the HCL. I will learn more about each method, as I have plenty of gold plated material to work with. I'm just wondering how to process this batch, for my first time, safely and quickly, so that way, by reading up on other methods, I can have a better understanding and can try other methods to see which works better for me.

Right now, the powder haven't dissolved, so, I'm needing to rethink what I need to do next. It's approximately 2 hours now since I added bleach and heat to the HCL.


Kevin
 
Palladium said:
Best $35 you will ever spend. You can heat these any way you want to. I have even used a blow torch on these things.
http://www.ebay.com/itm/Lot-of-5-Corning-Ware-Blue-Cornflower-Bake-Dishes-PYROCERAM-Modern-made-USA-/200886377657?pt=LH_DefaultDomain_0&hash=item2ec5c2dcb9
I'm going to look into buying some Corning Ware too. I see they do hold up good to flames and heat. I guess they're more of a ceramic than glass.

Thanks for the info.

Kevin
 
testerman said:
The dish IS a Pyrex. I confirmed it after checking on the powder.

I do have a more dishes I can put that in. I have been looking for one of the hot plates that's solid all the way around. I do like them better too, and I've seen more people using them than the kind I'm using. I'll upgrade soon. I'm also going to transfer everything in my beaker, then put the beaker in that dish (with some water added) to make sure that if the beaker breaks, it'll be contained in the pyrex dish.
Corning's Pyroceram and Visions cookware are the only kitchen glass suitable for stove top use. The pyrex dish you have is only suitable for oven use. It is not recommended for stove top use, whether or not there is any liquid in it.

What comes to mind is that there are different methods of doing this, and from the Tutorial I've been reading, I should be using Nitric Acid along with the HCL to dissolve the powder, yet, others use bleach with the HCL. I will learn more about each method, as I have plenty of gold plated material to work with. I'm just wondering how to process this batch, for my first time, safely and quickly, so that way, by reading up on other methods, I can have a better understanding and can try other methods to see which works better for me.

Right now, the powder haven't dissolved, so, I'm needing to rethink what I need to do next. It's approximately 2 hours now since I added bleach and heat to the HCL.
2 hours seems too long. Aqua regia (HCl + HNO3) is much faster than HCl / Bleach, but for powders, the HCl / bleach should still work.

Have you tested your solution with stannous to see if you have any gold in solution?

How much HCl and how much bleach have you used? You may need to add more of one or both.

As resabed suggested, the remaining powder may be other materials that were dissolved into your cell as you were getting it tweaked. Copper comes to mind as you mentioned your basket was suffering some degradation.

If your solution tests positive, I would be tempted to let it settle, then decant the pregnant solution to another beaker. Then add some fresh acid to the remaining solids and add some fresh bleach. Then test the new solution.

Hope this helps,
Dave
 
If it's good enough to go on the tip of a missile i will use it any day. :mrgreen:
http://www.corning.com/lifesciences/us_canada/en/technical_resources/product_guid/shp/pyro.aspx
 
FrugalRefiner said:
testerman said:
The dish IS a Pyrex. I confirmed it after checking on the powder.

I do have a more dishes I can put that in. I have been looking for one of the hot plates that's solid all the way around. I do like them better too, and I've seen more people using them than the kind I'm using. I'll upgrade soon. I'm also going to transfer everything in my beaker, then put the beaker in that dish (with some water added) to make sure that if the beaker breaks, it'll be contained in the pyrex dish.
Corning's Pyroceram and Visions cookware are the only kitchen glass suitable for stove top use. The pyrex dish you have is only suitable for oven use. It is not recommended for stove top use, whether or not there is any liquid in it.

What comes to mind is that there are different methods of doing this, and from the Tutorial I've been reading, I should be using Nitric Acid along with the HCL to dissolve the powder, yet, others use bleach with the HCL. I will learn more about each method, as I have plenty of gold plated material to work with. I'm just wondering how to process this batch, for my first time, safely and quickly, so that way, by reading up on other methods, I can have a better understanding and can try other methods to see which works better for me.

Right now, the powder haven't dissolved, so, I'm needing to rethink what I need to do next. It's approximately 2 hours now since I added bleach and heat to the HCL.
2 hours seems too long. Aqua regia (HCl + HNO3) is much faster than HCl / Bleach, but for powders, the HCl / bleach should still work.

Have you tested your solution with stannous to see if you have any gold in solution?

How much HCl and how much bleach have you used? You may need to add more of one or both.

As resabed suggested, the remaining powder may be other materials that were dissolved into your cell as you were getting it tweaked. Copper comes to mind as you mentioned your basket was suffering some degradation.

If your solution tests positive, I would be tempted to let it settle, then decant the pregnant solution to another beaker. Then add some fresh acid to the remaining solids and add some fresh bleach. Then test the new solution.

Hope this helps,
Dave
I tested the solution with stannous, and the q-tip turned completely black. After 3 minutes, it's still completely black. So, there is gold in the solution. The solution is between a dark yellowish/greenish color. But on the q-tip, the solution is yellow.

I first added 70 ml of HCL yesterday, then today I added approximately 50 ml of bleach. Then I added about 30 ml more HCL to make it a total of 100 ml.

So, what I'll do is decant the solution, then add "just bleach to the solids/powder"? If there is still gold in there, how will I know by just adding bleach? Would I need to add HCL + Nitric to let it dissolve the solids?

So far, I feel alot of progress is being made, because of the help I'm receiving, plus the understanding I'm gaining as I go along. This is very interesting to do.

Kevin
 
Palladium said:
If it's good enough to go on the tip of a missile i will use it any day. :mrgreen:
http://www.corning.com/lifesciences/us_canada/en/technical_resources/product_guid/shp/pyro.aspx
Nice... Very Nice! I gotta get me some. I know some are at the GoodWill store here. I'll definitely look for some of them.

Thanks

Kevin
 
The yellow solution is gold chloride (the green in it is copper chloride), let what you have sit, until the solution clears (no murky look to solution) decant the clear yellow (slight green) filter this liquid to a clean vessel, let this vessel sit in the sun to help drive off free chlorine, we will precipitate gold in this vessel later.

The remaining powders which may contain undissolved gold add more HCl acid, add a little bleach and stir, let powders react, as the chlorine is used up add some more bleach and stir again to dissolve more gold into solution.

We need to keep the solution acidic to dissolve the gold (as stated earlier bleach will raise the pH towards neutralizing the solution), you can monitor pH, or just make sure you have excess HCl acid in solution.

Note also before precipitating the gold we will need to be sure we do not have free chlorine in solution, here is where heating, or sitting in the heat of the warm sun can help to drive off the free chlorine out of solution before trying to precipitate your gold.
 
butcher said:
The yellow solution is gold chloride (the green in it is copper chloride), let what you have sit, until the solution clears (no murky look to solution) decant the clear yellow (slight green) filter this liquid to a clean vessel, let this vessel sit in the sun to help drive off free chlorine, we will precipitate gold in this vessel later.

The remaining powders which may contain undissolved gold add more HCl acid, add a little bleach and stir, let powders react, as the chlorine is used up add some more bleach and stir again to dissolve more gold into solution.

We need to keep the solution acidic to dissolve the gold (as stated earlier bleach will raise the pH towards neutralizing the solution), you can monitor pH, or just make sure you have excess HCl acid in solution.

Note also before precipitating the gold we will need to be sure we do not have free chlorine in solution, here is where heating, or sitting in the heat of the warm sun can help to drive off the free chlorine out of solution before trying to precipitate your gold.
Before you made this post, I had already added the smb after doing a stannous test. Below are some pictures I took just a few minutes ago.

stannous-test-result-01.jpg

smb-pre-drop-01.jpg

smb-drop-01a.jpg

I can see some black buildup on the bottom (sorry I didn't take a picture of it), but the sediment from the SMB is what I see most of. I believe I used approximately 10 tsp of SMB, slowly, 1 tsp at a time until it started to change. Did I add enough? Every time I add some (1 tsp at a time) it fizzles in the solution. It started getting dark outside, so I put it up, not knowing if I actually finished the dropping of the gold.

It's getting windy outside, although it's around 65F, they are predicting heavy rain tonight, and possibly tornadoes.

I'm going to do something to somebody if it blows all my stuff away. :twisted: It's in my drawer and closed.

Once I get one method of what I'm doing down-packed, I'm going to do it again to make sure I'm doing it correct, then I'm going to learn more on other methods of doing the same thing and determine which is better for me.

Once again, I love you all for all the help you've been providing, and it's been a "Never forgetting Experience".

Kevin
 
The green solution has a lot more copper mixed with your gold than I suspected.

Remember if you have free chlorine your gold will redissolve, which can create a problem of using too much SMB to try and precipitate the gold.

Use the stannous chloride test to determine when you have enough SMB and the gold has preciptated from solution.

The Picture after SMB looks to have undissolved salts, and the color is closer to what I would expect to see a gold solution without copper, I also see no green from copper in solution, if this is the same solution, it looks like you also precipitated the copper, things are not looking right here, you may have used way too much SMB.
 
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