Look at this thread http://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t=17070&hilit=sulfur+dioxide+generatorJHS said:
Göran
AMD Opteron 2212 for Noob
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Göran
rjamjb
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Latest update and a couple of questions.
Bye the way Göran, that bumper could have looked fantastic, pity he didn't manage to get all of it done.
Here is a wrap up of where things are just now.
This is the paper after filtering the Chloroauric acid through. The paper is slightly yellow as it evidently absorbed some of the Au2Cl6 so I’m keeping that (will need to work out what to do with my filter papers I’m keeping at a later date). I’m not sure whether the filtrate is worth keeping – some bits of shiny/glassy silica evidently in there but I’m not sure what else. A very fine silvery/grey dried substance as you can see.
The second picture is the sum-total of everything so far. You can see the Chloroauric acid on the left. The two Florence flasks contain HCL that had been used to wash the results of the AP a couple of times after filtering that from the original chips. On the right are three bottles (yes I am waiting for some labels to be delivered so it is clear that these contain chemicals, at the moment they are kept well out of the way in my garage). These contain the Cuprous Chloride left over from my AP/bubbling of the chips.
When I do another AP batch, I intend to add the HCL washes to the CuCl to help kick start it with the new batch of recovery materials. Hopefully I won’t need to use any H2O2 if I’ve already got the CuCl to start it off, just an oxygen bubbler.
Third and fourth pictures are of Sulfamic Acid and Tin Chloride (Stannous Chloride) Crystals.
This is how I intend to proceed.
Firstly
Make some Stannous Chloride testing solution (I will make the bare minimum I can as I won’t have large quantities to test over the forthcoming months/years )
Add two grams of SnCl2 into a small vial/glass tube. Add two to three mills of H2O. Then add HLC *I have 36% conc), about 7-10 mils to start (then one to two drops a time after that). Keeping the vial under a hot running tap, agitate/mix/dissolve the SnCl2. Keep adding HCL until all crystals are dissolved.
Use a drop of each of the three liquids (see pic) on a white tissue followed by a drop of the stannous solution to test for gold. I’m sure that I have the Au2Cl6 in the left hand jar. This is more as a test of principle and to give me some practice on uses of the Stannous.
Secondly
I suspect that I have around two grams of Au in the Chloroauric Acid and I used 50ml of HCL to make the Aqua Regia (I know, far too much – one mistake I won’t make again)– on a simple calculation I’ll have somewhere between 45-50 mils of the HNO3 to neutralise before I can move to drop the gold out of solution.
Dissolve 75grams of the Sulphamic acid in HCL (or would H2O be just as good?, or just mixing directly into the solution without dissolving?) until fully dissolved and then add a few ml at a time to the auric acid until no further reaction. 75 grams is on the basis that it will take approx. 1.5g of Sulphamic acid to rid 1ml of Nitric acid out of the solution. After this move to SMB.
Any thoughts or comments on these next steps/approaches?.
Regards - Russell
Bye the way Göran, that bumper could have looked fantastic, pity he didn't manage to get all of it done.
Here is a wrap up of where things are just now.
This is the paper after filtering the Chloroauric acid through. The paper is slightly yellow as it evidently absorbed some of the Au2Cl6 so I’m keeping that (will need to work out what to do with my filter papers I’m keeping at a later date). I’m not sure whether the filtrate is worth keeping – some bits of shiny/glassy silica evidently in there but I’m not sure what else. A very fine silvery/grey dried substance as you can see.
The second picture is the sum-total of everything so far. You can see the Chloroauric acid on the left. The two Florence flasks contain HCL that had been used to wash the results of the AP a couple of times after filtering that from the original chips. On the right are three bottles (yes I am waiting for some labels to be delivered so it is clear that these contain chemicals, at the moment they are kept well out of the way in my garage). These contain the Cuprous Chloride left over from my AP/bubbling of the chips.
When I do another AP batch, I intend to add the HCL washes to the CuCl to help kick start it with the new batch of recovery materials. Hopefully I won’t need to use any H2O2 if I’ve already got the CuCl to start it off, just an oxygen bubbler.
Third and fourth pictures are of Sulfamic Acid and Tin Chloride (Stannous Chloride) Crystals.
This is how I intend to proceed.
Firstly
Make some Stannous Chloride testing solution (I will make the bare minimum I can as I won’t have large quantities to test over the forthcoming months/years )
Add two grams of SnCl2 into a small vial/glass tube. Add two to three mills of H2O. Then add HLC *I have 36% conc), about 7-10 mils to start (then one to two drops a time after that). Keeping the vial under a hot running tap, agitate/mix/dissolve the SnCl2. Keep adding HCL until all crystals are dissolved.
Use a drop of each of the three liquids (see pic) on a white tissue followed by a drop of the stannous solution to test for gold. I’m sure that I have the Au2Cl6 in the left hand jar. This is more as a test of principle and to give me some practice on uses of the Stannous.
Secondly
I suspect that I have around two grams of Au in the Chloroauric Acid and I used 50ml of HCL to make the Aqua Regia (I know, far too much – one mistake I won’t make again)– on a simple calculation I’ll have somewhere between 45-50 mils of the HNO3 to neutralise before I can move to drop the gold out of solution.
Dissolve 75grams of the Sulphamic acid in HCL (or would H2O be just as good?, or just mixing directly into the solution without dissolving?) until fully dissolved and then add a few ml at a time to the auric acid until no further reaction. 75 grams is on the basis that it will take approx. 1.5g of Sulphamic acid to rid 1ml of Nitric acid out of the solution. After this move to SMB.
Any thoughts or comments on these next steps/approaches?.
Regards - Russell
rjamjb
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A few more pics to show progress.
At this point I just tested the AuroChloric acid - To my inexperienced eye this looks like a positive reaction. Agree?
I admit at this stage I did not measure the constituents of the Stannous Chloride very carefully. I added a few grammes of crystals, then a few mils of water. Then I added a few mils of HCL and agitated, then added again until the crystals dissolved. That was it.
The Crystal Stannous II Chloride in the pippette bottle
A few mills of H2O
After adding HCL
The TEST !!!
(Edit - bye the way is it "Chloroauric Acid", or "AuroChloric Acid" - I'm sure I've seen both uses)
At this point I just tested the AuroChloric acid - To my inexperienced eye this looks like a positive reaction. Agree?
I admit at this stage I did not measure the constituents of the Stannous Chloride very carefully. I added a few grammes of crystals, then a few mils of water. Then I added a few mils of HCL and agitated, then added again until the crystals dissolved. That was it.
The Crystal Stannous II Chloride in the pippette bottle
A few mills of H2O
After adding HCL
The TEST !!!
(Edit - bye the way is it "Chloroauric Acid", or "AuroChloric Acid" - I'm sure I've seen both uses)
Where is the violet color purple of Cassius, the reaction of gold in solution with stannous chloride?
Just because you see a reaction (or color change) does not necessarily mean you have a positive reaction for precious metals or gold, other metals in solution can react.
I would expect violet color or so dark of concentration of violet that it looks dark brown to black with a gold solution.
Here is another place where Hokes book and the getting acquainted experiments can help you gain a better understanding.
Just because you see a reaction (or color change) does not necessarily mean you have a positive reaction for precious metals or gold, other metals in solution can react.
I would expect violet color or so dark of concentration of violet that it looks dark brown to black with a gold solution.
Here is another place where Hokes book and the getting acquainted experiments can help you gain a better understanding.
rjamjb
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Thanks Butcher,
I thought that I could detect some purple/violet in the browner main color which is why I thought I had a positive. Mind you, looking at the picture again this is quite subtle and perhaps I am guilty of a biased view.
The paper with its dimples etc doesn't help to much in terms of clarity. I'll try again tomorrow with a filter paper which should be a bit more conclusive, I hope.
Russell
I thought that I could detect some purple/violet in the browner main color which is why I thought I had a positive. Mind you, looking at the picture again this is quite subtle and perhaps I am guilty of a biased view.
The paper with its dimples etc doesn't help to much in terms of clarity. I'll try again tomorrow with a filter paper which should be a bit more conclusive, I hope.
Russell
rjamjb
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Göran, I have taken a step backwards from my previous post and will follow your advice on reducing the solution via evaporation (then add HCL then further evaporation etc) to avoid adding too much Nitric reducing, additional chems into the solution prior to precipitation of the Au.
I will spend a little time with the stannous wondering why I'm not getting a very purple/violet colour also because I know there is gold in that solution having seen it dissolve!!. Perhaps a few more crystals of stannous II chloride in the current stannous testing solution might help also.
Bye the way Göran, I am in the UK and the weather is getting colder (but probably not as fast as it is for you!!!!) so evaporation through waiting naturally will take a long time so am purchasing a very cheap hot plate, hopefully to speed the evaporation up.
st
Will add a very minor amount of Sulphamic acid at the end just to "mop up" any final amounts of nitric but only minor amounts. Perhaps a gramme or two grammes only, hopefully not really needed.
I have to say, I am so tempted just to "drop whatever" I can and can't really wait to try it,...... but will wait accordingly until the time is right.
Can't wait to get to the final stage and 'drop' that gold, just gotta be patient!!!... (Message to self...... calm down and take it easy bro !!!!) Göran I'm gonna get the bug for 'dropping' soon !!!!
Russell
ps
Bye the way I have been researching how to deal with the lids of the original AMD chips I purchased (I've been dealing with the gold spots on the fiber parts in this thread but you will see that the lids to my CPUs have a gold plating also)- see original pics/posts - I'm still thinking a electro solution will be best. I think that this will be my next post.
pps
I have spent this evening re-reading the safety section of this site (If anyone is reading this thread then the safety sectiono IS A MUST!!!). If anyone is in any doubt about what I have done so far and has any doubt about what they are doing.... DON'T.
Regards all
Russell
ps - Kudos points to anyone who identifies and pinpoints where/what/why/how my avatar comes from?!!!
I will spend a little time with the stannous wondering why I'm not getting a very purple/violet colour also because I know there is gold in that solution having seen it dissolve!!. Perhaps a few more crystals of stannous II chloride in the current stannous testing solution might help also.
Bye the way Göran, I am in the UK and the weather is getting colder (but probably not as fast as it is for you!!!!) so evaporation through waiting naturally will take a long time so am purchasing a very cheap hot plate, hopefully to speed the evaporation up.
st
Will add a very minor amount of Sulphamic acid at the end just to "mop up" any final amounts of nitric but only minor amounts. Perhaps a gramme or two grammes only, hopefully not really needed.
I have to say, I am so tempted just to "drop whatever" I can and can't really wait to try it,...... but will wait accordingly until the time is right.
Can't wait to get to the final stage and 'drop' that gold, just gotta be patient!!!... (Message to self...... calm down and take it easy bro !!!!) Göran I'm gonna get the bug for 'dropping' soon !!!!
Russell
ps
Bye the way I have been researching how to deal with the lids of the original AMD chips I purchased (I've been dealing with the gold spots on the fiber parts in this thread but you will see that the lids to my CPUs have a gold plating also)- see original pics/posts - I'm still thinking a electro solution will be best. I think that this will be my next post.
pps
I have spent this evening re-reading the safety section of this site (If anyone is reading this thread then the safety sectiono IS A MUST!!!). If anyone is in any doubt about what I have done so far and has any doubt about what they are doing.... DON'T.
Regards all
Russell
ps - Kudos points to anyone who identifies and pinpoints where/what/why/how my avatar comes from?!!!
An electric coffee maker makes a perfect evaporator. Old ones pops up in the trash now and then. I have three so far. Comes with a built in thermal switch so the solution doesn't boil but can dry out.
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=67&t=16197
You can use it for heating reactions too when I dissolved some gold, 3:rd picture ...
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=19840#p201989
Göran
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=67&t=16197
You can use it for heating reactions too when I dissolved some gold, 3:rd picture ...
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=19840#p201989
Göran
rjamjb
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Nice coupla links Goran. I've an old coffee maker in the loft I'm gonna hunt down.
Mean time I re did the stannous test on some filter paper, pic attached. First quarter, which is south-west my chloroauric acid. Second two the hcls from washing. finally my left over cucl. Very green. . Positive test on the auric acid!!! Yay.!! Nice purple de cassius I think!!
Russell
Ps, a close up on the auric test also.
Mean time I re did the stannous test on some filter paper, pic attached. First quarter, which is south-west my chloroauric acid. Second two the hcls from washing. finally my left over cucl. Very green. . Positive test on the auric acid!!! Yay.!! Nice purple de cassius I think!!
Russell
Ps, a close up on the auric test also.
