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Lou
ActiveMember
A discussion with a friend via gmail chat earlier today sparked my mind about high purity precious metals. Sprinkled throughout the
literature are methods for obtaining metals and compounds of exceptional purity.
Here is one such method that reliably produces 6N+ pure gold.
As I find methods, I will continue to post them. At the very least, some of us here may have academic interests.
Method for UHP gold:
All acids and reagents used must be of trace metal grade. Recommended is the Trace Metal line of products from J.T. Baker. Under
no circumstances should any metal containing object or apparatus contact the gold or solution; only aqua regia boiled quartz and
PTFE apparatus should be used.
Gold of 99,995% purity (20 g.) well rinsed in ether and then in HCl is dissolved in aqua regia in an 800ml. acid washed quartz jointed
flask, and the solution is concentrated to a thick syrup at 80 degrees Centigrade, removing the most part of the nitric acid. It is then boiled
5 times further and periodically 20 ml. of hydrochloric acid (4:1) is added to expel nitrogen oxides. The residue is taken up in 650 ml. of
hot 18.2 M water and digested until all soluble material is dissolved. It is then allowed to settle for eight days in a dustfree atmosphere,
preferably in a closed system. The precipitate consists of AgCl containing small amounts of Au, Pd, SiO2, etc. The gold solution is vacuum
filtered through a micron quartz frit via decanting (do not disturb the precipitate). This and all later precipitates are not worked up further
to obtain gold.
Gold refined by use of SO2 still contains some Pd, while that precipitated with oxalic acid contains Cu, Pb and other metals. Therefore both
of these procedures must be used to obtain gold of the desired purity. Ultra high purity sulfur dioxide is passed through the warm gold
solution (80C) obtained above; the gold precipitates quantitatively on careful neutralization with ammonia (1:1). The product is allowed
to settle overnight and the deposit of spongy gold is washed by decantation (7 times) with 200 ml hot 18.2 M water; it is then heated for
four hours on a steam bath with concentrated hydrochloric acid and washed free of acid with hot 18.2 M water. Then it is redissolved in
aqua regia in a quartz flask, the nitrogen oxides removed, filtered, and reduced. The entire procedure above is repeated seven times in
order to remove all Ag, Cu, Ni, Zn and Pb. It is no longer necessary for the gold solution to sit. The precipitated gold product is then
digested for 12 hours with ammonia (1:1), washed free of ammonia with 18.2 M water, heated for four hours on a steam bath with hot
concentrated nitric acid, and decanted. Ammonia (1:1) is again added and later removed by washing with 18.2 M water . The gold sponge
is dissolved in dilute aqua regia; after addition of HCl, the solution is concentrated by evaporation, diluted with UHP H 2O, decanted and
filtered.
The gold is precipitated by careful addition (there is a danger of foaming over) of small portions of powdered, UHP crystalline oxalic acid
(ACS grade may be resublimed twice). If the solution retains a yellow colour, it is carefully neutralized with ammonia and more oxalic acid
is added; the addition of the acid is continued until the solution remains colorless. The resultant gold sponge is again dissolved and
reprecipitated with oxalic acid. It is then Pdfree. Finally the gold is redissolved, precipitated with sulfur dioxide and heated with
concentrated hydrochloric acid, and washed with 18.2 M water. The residual traces of HCl are removed with ammonia and it is again
washed with UHP water. The product is transferred to a quartz dish and dried at 110C. Yield 7580%. The gold prepared in this manner is
spectroscopically and analytically pure (free of metallic Cu, Ag, Ni, Pd, Fe, Zn and Pt) and is above 99,9999% in quality.
LasteditedbyLouonDecember1st,2008,4:02am,edited1timeintotal.
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Firewalker
July30th,2008,10:48pm
P
Dang Thanks for the info, but for a novice backyard operation like I have, Lazer Steve, here I come.
Seriously, that is real good information for the professional and novice, I even learned a couple of things from reading that (this old dog
can learn a few new tricks.)
But, what is 18.2 M Ohm water?
Luck....Jack
o
Noxx
SiteAdmin
July30th,2008,11:17pm
P
goldsilverpro
ActiveMember
July30th,2008,11:38pm
P
Good info, Lou. I can see a few of those things that I could incorporate into my procedure.
lazersteve
ActiveMember
Lou,
Great post, it reads like it came right from the Organic Synthesis site that I love so much!
18 Mega Ohm water is water that has a resistance of 18 Million Ohms on your ohm meter. Pure water free of dissolved solids has a very high
electrical resistance.
Steve
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Lou
ActiveMember
July31st,2008,3:20am
P
Water of that quality is very hard to make. It is really friggen pure water . The machine to make that water costs (or used to) about $8k,
oh and did I mention that it likes to break down and that you need to replace cartridges on it. Water that pure is a pain in the butt to
makemultiply distilled deionized water that's been passed over all sorts of ion exchange resins, activated carbon, assorted membranes,
and then repeated. Unfortunately, if you left such water in an untreated glass bottle or out in the open air, it would be ruined! It would be
basic from reacting with terminal hydroxys on the glass surface, and if exposed long enough to the atmosphere, it will become acidic from
absorbing CO2. Now you see why analytical chemistry is somewhat challengingvariables, and lots of them!
I love the uncanny resemblance this technique's rinse procedure has to that advocated by Harold, Chris, Steve, and used by many, many
more on this site!
I recently purchased some gold and platinum of 6N5 quality at spot price. Some of you may be thinking that it's a rip off, but gold from a
supply house refined by a chemist to that level of purity would command three times the market value per ounces in bulk. For small
amounts like 520g it would be 8 or more times market value.
As you may have noticed, the starting material was already purer than the quality of commercially pure gold (as Chris and Harold have
corrected me) at 99,995 so you can see the trouble that is required just to make a couple orders of magnitude purer. This procedure is one
I typed by hand (I had it loose leaf) onto the forum and it's fairly old (20 years at the least). I'm willing to bet that the procedure will give
gold of even higher purity than 6N, which was probably the limit of the most complicated analysis back then.
I also had/have procedures for rhodium, palladium, platinum, rhenium, osmium, ruthenium, and iridium. I suppose they're not useful from
the aspect of recovery, but they are highly useful as far as refining goes.
I think these procedures are enlightening just from the standpoint of it being the pinnacle of refining let alone from practical value it has
for us as refiners in improving our technique.
As I find them, I will post them. Moderators willing, perhaps we can move them into another thread and sticky it for future reference.
Lou
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Allthatglittersisnotgold.Occasionallyit'srhodium
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Noxx
SiteAdmin
July31st,2008,3:51am
P
I suppose another moderator stickied this post, it's not me this time
You're right Lou. The distilled/filtered water we use at our school lab has a pH aroud 5.5 if I remember correctly. This is due to dissolve
CO2 of course.
I'm glad you posted the process. In my never ending goal to reach to purest gold possible, this is very useful.
Cheers
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lazersteve
ActiveMember
Stickied Post
July31st,2008,3:55am
P
Lou,
I stickied the post for you.
Steve
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RagandBone
ActiveMember
August5th,2008,8:51pm
P
It would be cool if somone was setup for the ultra purity process. Everyone could send in their gold and do one big batch of it.
Unfortunately, it's beyond my technical ability.
"IprefervirginterritorybutI'lltakesloppysecondsanyday."
o
Lou
ActiveMember
August6th,2008,12:14am
P
I'm setup for it. It's just expensive for reagents, very, very expensive.
Likechemistry?Tryhttp://sciencemadness.org/talk
Allthatglittersisnotgold.Occasionallyit'srhodium
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hasoviboy2000
September19th,2008,5:58am
P
Lou,
Great post! but what if I'm happy with 4n's plus only. Is there any way I could refine scrape gold without costing me too much money and
time? Can I cut some corner with your procedure above? Can you post a procedure to get 4n's plus. thanks
o
Lou
ActiveMember
September19th,2008,11:34pm
P
Absolutely. Really, a good investment is dibutyl carbitol, a polyether that solvates gold. Diethyl ether also works, but you'll get one hell of
a buzz working with it in an unventilated environment. Its flammability also makes gasoline look benign.
If you just want to precipitate the gold once and get 4N, extract with dibutyl carbitol (nicknamed diglyme). Wash the extract well with 3M
HCl until it the acid is colorless. Then precipitate with the reductant of your choice. Filter and collect the gold, washing well with solvent.
Take the gold powder and (if rinsed right, it's chloride free) boil it with 4M nitric acid for an hour. If the nitric is colorless (no green, no
blue) then chances are good that you're doing well. Filter again (saving the nitric to use for some other purpose) and add the gold to
concentrated ammonia and stir for an hour or so. Any blue will indicated copper. You don't really need to rinse the gold after this, any
ammonia or ammonium nitrate will be lost to the melting process. The gold will assay 4N and it should take less than 6 hours from
dissolution of crude material to casting the pure metal.
Lou
LasteditedbyLouonSeptember20th,2008,6:54am,edited2timesintotal.
Likechemistry?Tryhttp://sciencemadness.org/talk
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Noxx
SiteAdmin
September20th,2008,1:36am
P
Lou wrote:
Anyway, I really like how DBG works. It's clean and efficient, and it's reusable !
Thismonthsraffle:
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Ifyouwanttosupportthisforumandalsogetridoftheads,membershipprogramsareavailableforyou!
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=62&t=24188
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Platdigger
ActiveMember
September20th,2008,3:13am
P
That last post was excellent Lou! I am saving that one for sure....
Randy
o
Lou
ActiveMember
September20th,2008,6:59am
P
Allthatglittersisnotgold.Occasionallyit'srhodium
o
Catxyoli
Member
hi everyone , i was searching the forum and found an excelent article betwen HaroldV and GoldsilverPro is astonishing and will shore clear
many minds on refining gold to 9.999
Please read especialy Goldsilverpro method
http://goldrefiningforum.com/phpBB3/vie ... y&start=15
good reading...
o
ppoowweerr
Member
So if someone were actually able to produce 6n or better gold, where or how would you sell it? I have not made any but I might pursue it in
the future if it became a practical option, although very unlikely.
o
Lou
ActiveMember
Semiconductors and specialty research purposes. It's not a commodity at that point by any measure.
Likechemistry?Tryhttp://sciencemadness.org/talk
Allthatglittersisnotgold.Occasionallyit'srhodium
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Noxx
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Thismonthsraffle:
http://goldrefiningforum.com/phpBB3/viewforum.php?f=60
Ifyouwanttosupportthisforumandalsogetridoftheads,membershipprogramsareavailableforyou!
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=62&t=24188
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Chumbawamba
ActiveMember
Holy wow, this is like the Olympic Gold Medal of refining. Has anyone here ever performed the process?
Who came up with it? Does it really require all those steps? I'm sure the answer is, "Yes, if you want 6N fine gold". What I'm interested in
knowing is the WHY for each step. For you experienced refiners each step probably makes sense, but for newbs like me I'm interested in
knowing what the chemical reasons are for each step. If some has the time to summarize I'd appreciate that. Otherwise, I guess I'll learn in
time.
o
Lou
ActiveMember
Who? It's a German procedure, I don't know who, but it's quite similar to that in Georg Brauer's collection but it must be a newer
modification because the technology to analyze gold to that purity (which is practically at detection limits) didn't really exist til ICPMS
came into its own.
Sulfur dioxide by itself gives a high quality precipitate, but is prone to reduce copper (II) to copper (I) which we see as a whitegray
chloride. Any silver is removed by the decantation procedure and by filtering. In this case, the gold is already very pure, so any copper that
is inadvertently reduced will remain in the acidic solution as a chloro complex. Doing it over multiple times will ensure that all the copper
is removed. Any palladium present will be a ''rider'' with the gold that comes down. To remove that, oxalic acid is used. The ammonia is
used to adjust the pH to get complete precipitation.
Likechemistry?Tryhttp://sciencemadness.org/talk
Allthatglittersisnotgold.Occasionallyit'srhodium
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Chumbawamba
ActiveMember
Hey Lou.
I still can't say I understand all of it, but your explanatory paragraphs certainly help in bringing me closer. Thanks for taking the time.
o
HAuCl4
ActiveMember
Ferro in page 10 of their BDG document claim 6N gold purity can be achieved with a certain oxalic acid mole concentration in the reduction
phase. I don't know if that claim is true, but that may help cutting some corners and some costs to obtain UHP gold.
I'd love to read Lou's comments regarding that claim on page 10 of Ferro's document.
I imagine very specific extractants are also available for UHP Pt and Pd, and probably every other metal in the periodic table.
ATTACHMENTS
Gold_Recovery_Butyl_Diglyme[1].pdf
(2.55MiB)Downloaded124times
"PlatinumistheonlymetalfitforaKing".KingLouisXVofFrance
o
BGT
Member
So I have gold precipitate from a gold drop using SMB (sodium meta bisulfite) 75 grams smb to a 500ml AU cloride filtered solution.
How do you get it to a dry powder after this? (steps to dry powder) Also, I have tried to torch the precipitate directly after it settles for 24
hours and while still wet and it just turns into black beads. (borax and argoflux were added) Should there not be any flux or borax in the
melting dish? Which Step is missing?
Thanks.
o
Harold_V
ActiveMember
BGT wrote:
How do you get it to a dry powder after this? (steps to dry powder) Also, I have tried to torch the precipitate directly after it settles for
24 hours and while still wet and it just turns into black beads. (borax and argoflux were added) Should there not be any flux or borax in
the melting dish? Which Step is missing?
Thanks.
Read Hoke.
I saw no mention of any attempt to wash the recovered gold.
Why is that?
Harold
Youarewhatyouwrite.
Wisepeopletalkbecausetheyhavesomethingtosay.Foolstalkbecausetheyhavetosaysomething.
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lazersteve
ActiveMember
BGT wrote:
So I have gold precipitate from a gold drop using SMB (sodium meta bisulfite) 75 grams smb to a 500ml AU cloride filtered solution.
How do you get it to a dry powder after this? (steps to dry powder) Also, I have tried to torch the precipitate directly after it settles for
24 hours and while still wet and it just turns into black beads. (borax and argoflux were added) Should there not be any flux or borax in
the melting dish? Which Step is missing?
Thanks.
Did you confirm you had gold in solution with stannous chloride befroe adding all that SMB?
That's a lot of SMB unless you had several ounces of gold in the 500mL. Copper I chloride will precipitate with SMB if a lot of copper is
present in the solution when the SMB is added. Copper will turn black when the torch flame is removed.
It's likely you precipitated a combination of gold and copper I chloride, melted it and now have dirty gold beads. Try sanding the black
coating off of one of the beads with an emery board to see if it has a golden core. If not, it may all be copper and or base metals.
Steve
Steve
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BGT
Member
I started using a separatory funnel with BDG. Tested with Stannous Chloride from beginning to end. Gold was there. Followed and
separated 3 times with 32% hcl wash. Used oxalic in a magnetic stirrer for 5 hours at 85C. Placed contents in Buchner Funnel and got 3
filters worth of brown powder. Torched the powder/filter with a MAPP torch and got black rocks. Sanded the surface and saw shiny gold
underneath, but it is so embedded within the rock like substance that my question is what is the best way to free it up again? Should I place
the rocks in sulphuric? Should I AR it all over again?
Thanks.
Mark
o
lazersteve
ActiveMember
The black is oxides from the base metals you pulled over from not following the proper process. Your HCl wash was way too strong and your
pregnant solution was not diluted first.
Here's a step by step process that works for me:
** Process using BDG
Here's the general procedure:
1. Dilute the pregnant solution to 25% concentration (1 part solution to 3 parts water).
a. Filter/Settle & Siphon out any sediments that form.
2. Add a portion of the diluted pregnant solution to your clean funnel (500mL).
3. Add enough BDG to hold the expected gold in the pregnant solution (BDG holds ~50 gm/L max). 250 mL of BDG will can strip out
12.5 gm of gold maximum.
4. Stopper the funnel and vigorously shake for several minutes.
5. Let funnel sit to until the two layers completely separate. The top layer should not be cloudy. The patent mentions a centrifuge, this
would speed the separation greatly.
6. Funnel off the lower layer into a separate glass vessel.
7. Repeat with each portion of the solution until all the solution has been processed using the same batch of BDG (Up to the 12.5 gm
limit).
8. In a separate beaker mix a solution of HCl (Muriatic 31.5%= 10 Molar) with distilled water 20 parts water: 1 Part HCl.( 19 mL H2O
per 1mL HCl). You will need a total of 3 times the amount of BDG you used of this diluted acid. If you used 250mL of BDG you need
to mix up 750 mL of this rinse acid (712.5 mL H2O to 37.5 mL HCl). You will be running three rinses of equal volume to the BDG
(250 mL). I only used one rinse when I did my experiments. The better you rinse the cleaner your gold. The patent states three to
five rinses.
9. Add an amount of the diluted acid from the step above equal to the volume of BDG used to the funnel. If you used 250 mL BDG then
add 250 mL of the diluted acid.
10. Stopper and shake vigorously for several minutes.
11. Let separate as before and drain off the acid wash into a separate vessel ( not the same one as before ).
12. Repeat steps 911 two more times. You can combine the rinses in the same vessel.
13. Dissolve 90 gm Oxalic acid per 100 mL of distilled H2O. Use the formula Lou has posted here to determine how much you will need.
Place 250 mL (equal volume to BDG) of this solution in a 1L pyrex beaker with a magnetic stirring rod (not required). Put the beaker
on a hotplate. Heat to 80C and turn on the stirrer (if available) to a very slow speed. Oxalic acid is hazardous READ THE MSDS!! Here
is a link to some follow up on Oxalic acid use.
14. Carefully filter the BDG from the funnel into the 1L Pyrex beaker with the Oxalic acid warm.
15. Heat (with stirring) for 23 hours. The gold will drop as beautiful gold flakes or a fine brownish mud. The BDG will be clear when it
is depleted of gold.
16. Filter the gold out and wash with full strength hot muriatic acid.
17. The gold should be 99.9%+.
The above is a method I formulated and tested from the BDC patent.
Steve
LasteditedbylazersteveonJanuary26th,2011,5:59am,edited2timesintotal.
Reason:Addedsubstep
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BGT
Member
Thank you so much for the detailed BDG information! Already starting it right now.
Just a few quick questions. How do you rinse the filter paper with the hot muriatic acid? Do you leave the round filter paper in the buchner
funnel with the brown powder sediment on the paper and pour in hot muriatic acid into the buchner funnel, wait for it to drain and then
remove the filter paper out? After removing the filter out of the buchner funnel, Is it better to let the paper air dry or just torch it right
away, or scrape off the powder from the filter when it is dry?
Mark
o
lazersteve
ActiveMember
Mark,
You could do it the way you suggest or you can wash the gold into a beaker with a spray bottle and add the HCl then heat. Pour off the acid
after the color of the acid no longer changes any darker.
Steve
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