# help with digestion



## IGutYa (May 22, 2010)

Ok, so i made a sulfur cell to deplate the parts i been having trouble with & it worked wonderfully. but now i am stuck with 2 problems.

1) i have 2.37g of black gold dust that i cant get to dissolve into hcl+clorox hot or not.

2) the deplated parts have more gold inside of them. but i cannot get the outer metal to dissolve. ive tried H2SO4, AP, 30% H2O2 AP, HCl, & now Hot 70% nitric & RFNA and not one of them does a bit of damage to it.  a density test comes rather close to Ti, but have any of you known radio connectors to be made of gold plated Ti??

i also realized that using RFNA on Ti (if that is what it is) can produce a pyrophoric reaction. so i quickly canceled that one after about 5 minutes.

Now ive read that Ti has no effect to AR, however i know that AR will dissolve this metal (leaving behind gold foil). it is only Slightly magnetic (to a super magnet stack), and it is silvery like nickel.

could it be Stainless Steel? all that Hot Nitric did was clean it & deplate any remaining gold. not one bit of the base metal will go into solution & no red-brown NO2 gas is made.

any ideas on how to digest it so i can get the gold from within? i would rather not make ar just for that.

i thought i had read hokes book, but i had it mixed up with the Handbook of Chemistry. Ah simple mistake. so i am now reading the correct one. im about half way threw but i figured i would pop the question in here too just to be safe.

Thanks for the help.


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## shyknee (May 23, 2010)

Seems like you spent more money than the little bit of gold your after is worth.


> ive tried H2SO4, AP, 30% H2O2 AP, HCl, & now Hot 70% nitric & RFNA


truely knowing when to stop the chase could be considered part of refining . No?.....


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## IGutYa (May 23, 2010)

shyknee said:


> Seems like you spent more money than the little bit of gold your after is worth.
> 
> 
> > ive tried H2SO4, AP, 30% H2O2 AP, HCl, & now Hot 70% nitric & RFNA
> ...





perhaps, but all in all it is a Learning experience. you can only learn so much without doing.

really ive only uesd about $10 in chemicals so its not that big of a loss.


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## IGutYa (May 23, 2010)

30% h2o2 can be made by boiling 3% h2o2. so $3 worth (wally-world) boiled down is PLENTY.
RFNA costs about $15 per pound to make (that is $6 per lb of kno3 x2 + $5 per half gal of H2SO4)
then add a little water to make the 70% nitric ( 0 $ )
hcl is $3 a gallon at lowes

and i only used a total of 100ml RFNA, ~500ml HCl, ~800ml H2O2, and 300g of KNO3 (nitric distillation, got 150ml RFNA), putting me at less than $5 in chemicals.

honestly, i dont see the costs here?


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## Palladium (May 23, 2010)

Cost money to get an edu- ma- cation.


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## IGutYa (May 23, 2010)

Palladium said:


> Cost money to get an edu- ma- cation.



you can spend years being edu-ma-cated and never learn what you need to know. ive had a chemistry class & have a gen. chemistry book that i have read 3 times now. i also have a nice book on metallurgy, plus all your books (Forum). not to mention the Fact you dont need a chemical background to be a refiner. you learn by doing.

i can study all the books i can get my hands on, but until i go and DO, ill never have a good understanding.


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## shyknee (May 23, 2010)

what was your feed stock ( pictures would help )
then show us the feed stock after stripping 
did you manage to retrieve any gold at all from your HCL+clorox ?
how many pounds of feed stock did you strip?
these are good questions you will need to answer so that some good help can come your way?
my earlier comment " truely knowing when to stop the chase could be considered part of refining . No?....." was from something I learned early on.
good luck
stay safe


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## shyknee (May 23, 2010)

> however i know that AR will dissolve this metal (leaving behind gold foil).


No .AR will not leave behind gold foil.


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## IGutYa (May 23, 2010)

i started off with 1.102 lbs (500g) of plated parts. from that i got 2.37g black powder from the sulfur cell (external only). that black powder in hcl+clorox does nothing. hot or not. i did a stannous chloride test on the hcl/clorox & it was negative so i filtered the black powder to save & disposed of the hcl+clorox.

i understood your first comment. and i feel it. haha. but when i look at how much ive spent, it really dont hurt that bad (for now).

as for the pictures....

What i started with (not the full 500g):
http://www.mediafire.com/i/?mo1f0ynzhzj

Before & After Sulfur Cell:
http://www.mediafire.com/i/?mlnza2xzzzj
http://www.mediafire.com/i/?lj4trymnjnz
http://www.mediafire.com/i/?nztzzzdfhwr ( one is partially deplated )

After Sulfur Cell:
http://www.mediafire.com/i/?n4nwqjvogrl

Before & After showing inner Gold:
http://www.mediafire.com/i/?ngmojn3g2z4

Nitric washes:
http://www.mediafire.com/i/?yihllanzcvo
http://www.mediafire.com/i/?j2zzzigmifw


New & Post Acid Peroxide:
http://www.mediafire.com/i/?4wwd1c0gcvm


Now i did try AR before i made the sulfur cell as a means of deplating as AP & nitric had no effect on the New. the AR quickly digested the parts leaving me with a golden mud in the bottom of the AR (i managed to get a little sample of the mud too) & upon filtering i found the following:

After AR:
http://www.mediafire.com/i/?wozwgjmgni2

Before & After AR:
http://www.mediafire.com/i/?dndzlmmgjit

Foil after AR:
http://www.mediafire.com/i/?lzidqdxt0y2


The AR photos were of only 20 individual parts as a test run. first it was 20 in AP, then the same 20 in nitric, then added a little hcl to the nitric to make AR & that finally did it. which is what i am considering doing with the nitric leftover from the hot washes in the first photos, after filtering the gold foils first.


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## IGutYa (May 23, 2010)

shyknee said:


> > however i know that AR will dissolve this metal (leaving behind gold foil).
> 
> 
> No .AR will not leave behind gold foil.




see that is what i expected too. but there was foil left in the bottom. as seen in the photos.

i would imagine the AR was totally saturated by the time it reached the inner foil. since the outer foil was gone, i figured the brown mud was it & was pushed out by the base metal (still unsure as i lost this first bit due to bumping acid). the stannous chloride test was Positive here.


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## shyknee (May 23, 2010)

looks like nitric did leave you with foils after dissolving the nickel-plate(or silver-plate) the color of the nitric says nickel-plate.
with a spray bottle use distilled water to knock the foils free one by one.
then use AR on the foils.
use AR on the black powder from the cell.
500g of pins will have alot more gold than 500g of these connectors and you can expect the pins will produce about 1g this may give you an idea of the total out come(total gold to expect) of your experiments


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## IGutYa (May 23, 2010)

these are military radio connectors from india. the nitric wash was after running them threw the sulfur cell. what you see is the foil the sulfur cell missed. the first time i did a nitric wash on them (before the sulfur cell), they had no reaction to the nitric.

they are press fit together, and contain just as much gold on the inside as the outside. as all the parts are double side plated inside-and-out & press fit.

so far i have a total of 2.52g of black cell powder & foils. not counting what is in the nitric wash or the internal (estimated ~2.5g).

so if it is nickel, why wont it digest into the nitric? it will gladly digest if i add some hcl. the nitric shouldnt be saturated as it has only dissolved about 1g of metal, if that.

is AR the best way (at this point) to extract the inner foils? 
ill AR the foils & the black powder tomorrow, should i do them separate or will they be fine in the same batch of AR?


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## qst42know (May 23, 2010)

In your sulfuric stripping cell what concentration of sulfuric acid were you using?

If using AR on these it is important that all base metals be digested completely. The crusty coating on the remains you show is likely much of your gold. Foils remaining after AR indicates that one or the other of your acids were depleted. 

From your photos I see you are working in a canning jar this is risky as some chemical reactions can create enough heat to break these. 

Nitric acid, HCL/Cl, and AR, any of these solutions will work better when you can heat them. A second hand glass coffee pot in good condition is a better choice to process in. Then perhaps you can run some of your processes to completion. 

I feel you are going in many directions with these but missing some of the important fine points.


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## Barren Realms 007 (May 23, 2010)

IGutYa said:


> these are military radio connectors from india. the nitric wash was after running them threw the sulfur cell. what you see is the foil the sulfur cell missed. the first time i did a nitric wash on them (before the sulfur cell), they had no reaction to the nitric.
> 
> they are press fit together, and contain just as much gold on the inside as the outside. as all the parts are double side plated inside-and-out & press fit.
> 
> ...



Since you added yourlittle bit of HCL to your nitric you might have hard time getting rid of all your nitric to recover your gold. 

I feel it will be easier for you to stick to the HCL/Clorox road to disolve your powder and flakes. You might want to try HCL/calcium hypochlorite(pools shock) that way you are not diluting your HCL with the water from the clorox. Heat your solution to about 140F and slowly add the dry chlorine, stirring constantly. You will think your getting now where but then you material will go into solution. Make sure you let it set in the sun to burn off the excess chlorine when you are finished. 

I don't know if this will work but years ago I soaked some 3/4" 316 SS bolts in some HCL, I forgot about them for a few days and when I came back to them the HCL had eaten the chromium out of the bolts leaving very light swiss cheese looking bolts.


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## shyknee (May 23, 2010)

qst24know
I found IGutYa's statement perplexing


> i started off with 1.102 lbs (500g) of plated parts. from that i got 2.37g black powder from the sulfur cell (external only). that black powder in hcl+clorox does nothing. hot or not. i did a stannous chloride test on the hcl/clorox & it was negative so i filtered the black powder to save & disposed of the hcl+clorox.


Thank for your help on this " that black powder in hcl+clorox does nothing. hot or not "


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## qst42know (May 23, 2010)

It seems to me, (and this may only be my perception) Igutya is rushing all these processes, and running none to completion.

It is difficult to find a solution when so many directions are pursued at once.


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## kdaddy (May 23, 2010)

I have ran hundreds of these RF connectors through the sulfuric cell and they never looked like yours do in the pic's. They allways came out a very uniform silver color due to the nickel plating under the gold. Please explain your cell setup, I'm thinking thats where
your problem lies.


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## qst42know (May 23, 2010)

Reverse polarity and acid concentration are two big issues to check.


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## IGutYa (May 23, 2010)

qst42know said:


> Reverse polarity and acid concentration are two big issues to check.




i set up the sulfuric cell just as lasersteeve's video's show. i used the same Roto drain cleaner (98% h2so4) with the same lead cathode (negative to battery charger) with the anode (positive) hooked up to each individual part as i couldnt get them to go as one big batch.

getting the parts to deplate with the sulfur cell was no problem.


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## IGutYa (May 23, 2010)

shyknee said:


> Thank for your help on this " that black powder in hcl+clorox does nothing. hot or not "




i tried first cold, then brought nearly to a boil & held. the end result was a yellowish-green acid that tests Negative for gold with stannous chloride & all the black powder sitting in the bottom.

i have no doubts that AR will be able to take care of it.


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## qst42know (May 23, 2010)

Boiling will destroy the chlorine which you need, as will direct sunlight. Chlorine will also dissipate with time.


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## Barren Realms 007 (May 23, 2010)

IGutYa said:


> shyknee said:
> 
> 
> > Thank for your help on this " that black powder in hcl+clorox does nothing. hot or not "
> ...





This is a tread from Steve.


I'm going to assume this black (?) material is from a sulfuric stripping cell.

Here's how I would proceed from this point forward.

1. Rinse the entire contents of the filter into a straight walled beaker and cover the black sediment with HCl to twice it's thickness in depth.

2. Heat to 60C.

3. Add 10 mL of Clorox and stir until the solution no longer fizzes with tiny bubbles.

4. Repeat Clorox additions with vigorous stirring after each until color of sediment changes from black to a tan/light brown/gray or completely dissolves, whichever comes first.

5. Test solution with stannous chloride for gold.

6. Do a coarse filtration on the the liquid to remove the bulk of the sediment.

7. Thoroughly rinse the sediment in the filter.

8. Perform a final fine filtration through a vacuum filter paper and a frit or with a charmin plug.

9. Heat the filtered solution on low heat to drive off any excess chlorine.

10. Add SMB to precipitate the gold.

If the material is not from a cell I may proceed differently.

Steve


Sounds like you either typed this backwards from my instructions or performed it backwards, I will assume it's a typo as you should add the HCl to the powder first, then slowly add small increments of Clorox. You may have to add more HCl if a small fresh addition of Clorox does not produce any reaction and there is still visible gold, black powder, or brown powder present. Since liquid bleach is dilute (2.5-5%) right out of the jug, not much chlorine gas (the active ingredient) is formed with each addition, that's why the fizzing stops. Stirring allows the dilute Clorox to contact the HCl in the solution to produce the chlorine gas to dissolve the gold. Stirring also brings the powder off the bottom of the beaker and allows it to contact the chlorine. This is why stirring is so important. Not just a simple stir like you stir your coffee, but repeated vigorous stirring.


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## IGutYa (May 23, 2010)

Barren Realms 007 said:


> Sounds like you either typed this backwards from my instructions or performed it backwards, I will assume it's a typo as you should add the HCl to the powder first, then slowly add small increments of Clorox. You may have to add more HCl if a small fresh addition of Clorox does not produce any reaction and there is still visible gold, black powder, or brown powder present. Since liquid bleach is dilute (2.5-5%) right out of the jug, not much chlorine gas (the active ingredient) is formed with each addition, that's why the fizzing stops. Stirring allows the dilute Clorox to contact the HCl in the solution to produce the chlorine gas to dissolve the gold. Stirring also brings the powder off the bottom of the beaker and allows it to contact the chlorine. This is why stirring is so important. Not just a simple stir like you stir your coffee, but repeated vigorous stirring.




yea i mixed the hcl & clorox first then added the powder, then added more clorox, heated, added more clorox, more acid. Nothing. so i let it cool down & filtered the black powder, tested the liquid with stannous, which was negative. so i tossed the acid clorox & kept the powder. again i only used a small amount of powder (from the first sulfur cell run) as a test.

now i have 2.52g of black powder from the sulfur cell (not including first run) + ~1g in foils. Plus the gold still inside of the parts, which is about the same amount as the outside.

i am willing to have another go at hcl+clorox or hcl+pool shock (calcium hypochlorite). if all else fails i have the nitric for AR.

i am still wondering how to digest the rest of the parts to get to the inner gold? hot nitric has no effect, or anything else for that matter, except for AR. i would hate to throw away 2g of gold just because.

Thanks for all the help.


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## Barren Realms 007 (May 23, 2010)

Try the HCL/clorox as Steve suggests, you will be suprised how well following his guidence works.

Your remaining items I think I would boil them in water to remove any traces of acid and then roast them to remove any traces of acid or water and then try the cell again. What were you using for your power source for your cell?


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## IGutYa (May 23, 2010)

Barren Realms 007 said:


> Try the HCL/clorox as Steve suggests, you will be suprised how well following his guidence works.
> 
> Your remaining items I think I would boil them in water to remove any traces of acid and then roast them to remove any traces of acid or water and then try the cell again. What were you using for your power source for your cell?



i got a 10 amp battery charger set on manual. it never used more than 6 amps tho.

the parts are clean, externally. nice and shiny. except for a few specks here & there, nothing id put in the cell again for. it is the gold inside of them im after. they are press fit together & both sides of the press fit parts are plated, plus there is a plastic piece inside each one that is covering some gold plating too. the parts are clean and appear void of gold, but i have one that digested partially that you can see the inner gold ( http://www.mediafire.com/i/?nleaqiqzzjm ) plus the parts from the AR that didnt digest ( http://www.mediafire.com/i/?wozwgjmgni2 ) that show more foil that was missed. i did the math based on what i got from a test run of 20 parts and can estimate the internal gold content of being around 2.5g for the entire 500g.


New Photos After Hot Nitric wash:

nice and shiny:
http://www.mediafire.com/i/?4nedngom2ze

new / post sulfur cell / post hot nitric wash:
http://www.mediafire.com/i/?mzd5mw0mzzb

before & after:
http://www.mediafire.com/i/?w2znoqqo1y4

gold foil left behind after Hot Nitric wash:
http://www.mediafire.com/i/?ojnd4qmyzj5
http://www.mediafire.com/i/?wkzkr1zruqy


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## IGutYa (May 23, 2010)

i just found out that coffee pots are not necessarily the best thing to use. turned the heat on medium & was heatin some AR up, then just as i turned the heat down the bottom of the jar cracked & started leakin hot AR into my hotplate.

luckily i had a dish nearby to pour the hot AR into so i only lost a few drops. either way i about sh*t myself.


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## qst42know (May 23, 2010)

Even the best lab glass can give it up with little or no warning. It pays to be ready for anything. Bring plain water to a hard boil before you trust used coffee pots. Some will last a long time but others have been subjected to too much abuse in their normal life span.


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## IGutYa (May 23, 2010)

qst42know said:


> Even the best lab glass can give it up with little or no warning. It pays to be ready for anything. Bring plain water to a hard boil before you trust used coffee pots. Some will last a long time but others have been subjected to too much abuse in their normal life span.




yea i used it not much. i felt safer boiling with the pyrex bowl. im just glad it didnt all go at once and dump hot acid on my hotplate.

i heard it crack and thought ooh sh... then i saw it drip.... haha cat like reflexes.

these connectors are a serious pain in the ass. hell of a first time go. i shoulda tried plain pins or something simple. too bad its such an expensive hobby to learn.


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## butcher (May 23, 2010)

if a glass of solution cracks it is not a good idea to lift it, the bottom can fall out, you can remove contents with suction bulb, these are also good for transferring or adding solutions as well as decanting down to the last drop. catch basin under hot plate and on workbench can aid in holding spills, cafeteria fiberglass tray's work here.

http://www.google.com/imgres?imgurl=http://images.allegrocentral.com/A9/C1/50cc-ml-Irrigation-Bulb-Syringe-560327-MEDIUM_IMAGE.jpg&imgrefurl=http://www.allegromedical.com/syringes-c570/50cc-ml-irrigation-bulb-syringe-p560327.html&usg=__DLXtYhn9j6dRLpwsr8KTEioi-M4=&h=240&w=240&sz=6&hl=en&start=13&um=1&itbs=1&tbnid=D9i9HL0O0rrccM:&tbnh=110&tbnw=110&prev=/images%3Fq%3Dsuction%2Bbulb%2Bsyringe%26um%3D1%26hl%3Den%26sa%3DN%26tbs%3Disch:1

http://www.google.com/imgres?imgurl=http://www.1-hydroponics.co.uk/images/miscellaneous/middlesize/pipettes.jpg&imgrefurl=http://www.1-hydroponics.co.uk/miscellaneous.htm&usg=__cRQnFnNa_qRrVc5yPjrtH0KmoFM=&h=248&w=357&sz=11&hl=en&start=81&um=1&itbs=1&tbnid=6b1T7q2OlBuCxM:&tbnh=84&tbnw=121&prev=/images%3Fq%3Dsuction%2Bbulb%2Bpipette%26start%3D80%26um%3D1%26hl%3Den%26sa%3DN%26ndsp%3D20%26tbs%3Disch:1


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## gold4mike (May 25, 2010)

One thing that struck me while reading your post is that you mixed the HCl and Clorox, then added more Clorox. You tested the resulting solution for gold using stannous chloride and it showed negative. When you test the solution for gold you must ensure that all the chlorine has been gassed off by heating or by exposing to sunlight and/or open air, preferably overnight. If you hurry that step the solution will immediately redissolve your gold giving the false impression that you have a negative test. It's possible you tossed some or all of your values with the solution when it seemed to test negative.

I hope I'm wrong!


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## shyknee (May 25, 2010)

eveything one can possibly need to grow some good chronic .thanks for the link butcher :lol: :lol: :mrgreen:


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## IGutYa (May 25, 2010)

gold4mike said:


> One thing that struck me while reading your post is that you mixed the HCl and Clorox, then added more Clorox. You tested the resulting solution for gold using stannous chloride and it showed negative. When you test the solution for gold you must ensure that all the chlorine has been gassed off by heating or by exposing to sunlight and/or open air, preferably overnight. If you hurry that step the solution will immediately redissolve your gold giving the false impression that you have a negative test. It's possible you tossed some or all of your values with the solution when it seemed to test negative.
> 
> I hope I'm wrong!




thats a good tip, thanks. i weighed the black powder before & after putting it into the hcl+clorox & it was the same. when i put it in nothing happened. when i heated it, nothing happened. it felt rather disappointing. i still have about 3 grams of foil/black powder (from sulfur cell) that needs taken care of.

what color is the black powder usually After running it threw hcl+clorox??

btw i tried to AR the remaining parts to get the inner gold since nothing else would digest them, this time the AR failed. it barely digested anything. the first time it completely digested the very same parts. i even heated it this time!

what a mess.


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## shyknee (May 25, 2010)

gold4mike said:


> One thing that struck me while reading your post is that you mixed the HCl and Clorox, then added more Clorox. You tested the resulting solution for gold using stannous chloride and it showed negative. When you test the solution for gold you must ensure that all the chlorine has been gassed off by heating or by exposing to sunlight and/or open air, preferably overnight. If you hurry that step the solution will immediately redissolve your gold giving the false impression that you have a negative test. It's possible you tossed some or all of your values with the solution when it seemed to test negative.
> 
> I hope I'm wrong!


I agree with this .And now you have ether sliver chlorides(if they used silverplate and i think they did) or lead sulfates as your black powder never throw away any thing untill you have what you're after. 
also the term "to completion" is very important ,you may have to add more acid or oxidizer so you can go to completion


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