Gold not dropping - why is it my sulfamic?

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Poorman's AR works way better with heat. Adding sulfuric to small lots can raise enough heat to kick start the reaction without heat at times. Adding large amounts of sulfuric to small volumes can be very dangerous as well.
 
Alright, here is my end. I believe i got the gold this time BUT whst the heck is this crystal that formed? @Shark @Yggdrasil I think i may have added a bit too much SMB? I added like id like to say 5 grams for .05g recovery hahaha. Could this be the reason?
 

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See if hot water will dissolve it. if it does, decant it off or filter out your gold. Which ever works best for you. If it doesn't, go back to AR and drop again using what you now know as a better expection on weight. This will reduce the risk of it occuring again. For volumes this small a 100ml or 250ml beaker would be plenty large enough for the job. Drop with 1/2 to 1 gram SMB.

You can decant down to the material, then add water and heat to below boiling. See if that removes it.

You can filter and run hot water through the filter if that is easier as well. I used to do this with coffee makers by filtering out the material, put the filter and material back in the coffee maker and add water. Turn it on and wait till the hot water runs through. My guess is hot water will do the job.
 
Alright so this is my second time with expectation of very VERY low gold drop.

I did the following

1. 2x HCL baths waited 1 day each
2. Poor man Aqua Regia
3. Waited for rxn to stop
4. Add sulfamic until no reaction (just 2 pinches)
5. Tested and received positive reaction
6. I have a very dirty gold drop so i mixed a bit of HCl with SMB and poured into AR solution.
7. PH is now showing 1
8. Waiting a whole night to see what i can recover

Notes: Kept my side solution as i have gold per pictures

secondly my AR solution went from emerald Green now it is just looking brownish black. Any feedback this time around?

Additionally im getting a reaction when i drop SMB and some SO2 is coming up.
What is these two images?
 
What is these two images?
The first image is crystals that forumed with my smb drop. Turns out it was just lead chloride.

The second image is residual gold left over. This is telling me i probably did not make my poor mans aqua regia correctly.

So i researched and read hokes book again and i did not boil my sodium nitrate and hcl solutions until it was orange (only to the point of faint yellow) so now i am on my third gold drop attempt with 200g PROMs. And i think it is working the color went from light green/yellow to now the image attached. Ill wsit a day to see what i get.

I listened to All recommendations and i added more water at the end.

One thing though is that i had to use ALOT of SMB despite there being no Nitric (i believe i neutralised with sulfamic and left it to sit overnight)
 

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See if hot water will dissolve it. if it does, decant it off or filter out your gold. Which ever works best for you. If it doesn't, go back to AR and drop again using what you now know as a better expection on weight. This will reduce the risk of it occuring again. For volumes this small a 100ml or 250ml beaker would be plenty large enough for the job. Drop with 1/2 to 1 gram SMB.

You can decant down to the material, then add water and heat to below boiling. See if that removes it.

You can filter and run hot water through the filter if that is easier as well. I used to do this with coffee makers by filtering out the material, put the filter and material back in the coffee maker and add water. Turn it on and wait till the hot water runs through. My guess is hot water will do the job.
TBH Shark when I used to use SMB (which is a long time ago) I never worried about using too much. It washes out quite merrily.
 
It seems I need to stop using it as well. If I use very much or even around it much I start having bad leg cramps. Looks like copperas will be more reached for now days.
Okay so the color change was this very very black powder that was WAYY to fine to filter. I brouhg it to a boil for 2 hours. So my gold was lost again for the third time. I am so confused. I have dont really get it. I had the gold drop once before but i cannot do it and recreate it. Is it possible that if the pH is below 1 that could affect the recovery when adding SMB?

What is that fine dark powder that settles at the bottom but cannot be decanted?

Do i have to boil the AR prior to adding SMB for longer?

Note :There is no excess nitric as there is no reaction from sulfamic.

I tested stanneous multiple times and i have color change but i can never seem to get the gold to drop.

I have no idea what im doing wrong. The picture of the SMB shows im using sulfite (SMB) should i switch to using this?
 

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Okay so the color change was this very very black powder that was WAYY to fine to filter. I brouhg it to a boil for 2 hours. So my gold was lost again for the third time. I am so confused. I have dont really get it. I had the gold drop once before but i cannot do it and recreate it. Is it possible that if the pH is below 1 that could affect the recovery when adding SMB?
You do not loose Gold by having too low pH, if the pH is too high it may not work, that is all.
It is not possible to say if you have excess Nitric/NOx/Nitrate with the visible reaction on Sulfamic.
Is there any black in the powder before adding AR?
The Gold drop will not be true black, it may be a dirty blackish brown that is very fine, if it is a dirty and dilute solution.
Have you washed out any silt from the solution beofer you start leaching the Gold?

What is that fine dark powder that settles at the bottom but cannot be decanted? Any kind of silt and mud from the grinding

Do i have to boil the AR prior to adding SMB for longer? Not necessary to boil for the SMB

Note :There is no excess nitric as there is no reaction from sulfamic. There still may be, try cementing on Copper.

I tested stanneous multiple times and i have color change but i can never seem to get the gold to drop. How do you test with Stannous?

I have no idea what im doing wrong. The picture of the SMB shows im using sulfite (SMB) should i switch to using this?
Try cementing on Copper.
Comments in the quote in bold.
 
Comments in the quote in bold.
Hello! Thank you so much for the comments.

1. Regarding the excess Nitric ( I've added sulfamic on heat to check - there is no visible reaction)

2. It was crystal clear yellow green prior to adding SMB. There was no hint of brown in this color.

3. Prior to AR solution had been washed extremely thoroughly and it was cleaned.

4. Stannous test revealed no reaction. Prior to the SMB drop I was getting a very light purple color.
 
Hello! Thank you so much for the comments.

1. Regarding the excess Nitric ( I've added sulfamic on heat to check - there is no visible reaction)

2. It was crystal clear yellow green prior to adding SMB. There was no hint of brown in this color.

3. Prior to AR solution had been washed extremely thoroughly and it was cleaned.

4. Stannous test revealed no reaction. Prior to the SMB drop I was getting a very light purple color.
Then there is so little Gold you can not see it.
It will be in a very thin layer on the bottom next day.
 
When dropping from a dirty solution (to much copper for example) you get drag down contaminants making the gold look very dark. If your only expecting a tenth of a gram or so of gold you best accomplish this in 50ml to 100ml beakers.

What did your stannous show before and after turning dark?
 
When dropping from a dirty solution (to much copper for example) you get drag down contaminants making the gold look very dark. If your only expecting a tenth of a gram or so of gold you best accomplish this in 50ml to 100ml beakers.

What did your stannous show before and after turning dark?
Before SMB - very very light purple (which is in line with what youve mentioned)

After SMB - no color change
 
Before SMB - very very light purple (which is in line with what youve mentioned)

After SMB - no color change
That indicates the gold dropped. It could be so fine that you may not see it, or is just not enough time for it to settle. A quality filter with the right porosity should catch it. Often when a drop is dirty it will also be very fine making it hard to filter or very slow to settle. Patience becomes important when this happens and could be several days before fully settled. This happens often when working with very small amounts of gold as well. It can be annoying and cause one to try and rush things where slowing down is what is needed.
 
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