# too much NaNo3 as a prticipian?



## cvikatore (Oct 10, 2013)

having problem I put too much NaNo3 and got a lot of brown look like mud, what too do now?


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## maynman1751 (Oct 10, 2013)

You have to tell us more. What did you process, how much, what process, etc.?
Maybe the brown 'mud' IS your gold!


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## cvikatore (Oct 10, 2013)

OK, I dissolved about 20 ceramic CPU s, that is seven grams of gold in my calculation, in AR about half a liter. And didn`t all gold dissolved something was undissolved so never mind. After filtering and cooking AR to neutralized nitric acid (I think I made a mistake cooking only once, cause I thought that nitric all gone since the not all gold dissolved) And when the AR gone about 0,1 liter put water 0,5 liter, heated and put some sodium nitrate to participate and nothing hapend put sam more water and still nothing, my thinking was that id too much water so I cooked once more to reduce water and put same more sodium nitrate and still nothing and when i put on the heat again there was changed color from dark brown and yellow to muddy green and that mud was going slowely on the bottom and there it is I will send some pictures.


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## Harold_V (Oct 10, 2013)

Go back to reading Hoke's book. You clearly do not understand what you're doing. 

If, in the process of extracting values, you find undissolved metals, why would you expect that you have anything of value in the solution? Unless what you are dissolving is solid value, with no base metals present, any values that may have been dissolved will have been cemented by the remaining base metal. 

As I said, you need to return to reading. Without the basic understanding of how these processes work, you'll struggle endlessly, never knowing what you have, or why you have it. 

Read Hoke. Read Hoke again. Read Hoke until you UNDERSTAND what she teaches. 

Harold


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## maynman1751 (Oct 10, 2013)

What Harold said plus you certainly don't precipitate with sodium nitrate!!!!!!!!
Read and study all of the blue entries in my signature line below this comment.
You sure as hell aren't ready to be doing what you're doing.
You're going to end up hurting yourself or others. You're working with some mighty dangerous chemicals and processes here.
One wrong move and you could be seriously injured or killed!!!! NO B.S.!!!!


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## moose7802 (Oct 10, 2013)

I'm going to second and third what harold and maynman1751 said. What you have said is way off and you need to read. Why are you trying to drop something when you said that not everything had went into solution, that's a no no right off the bat. Also sodium nitrate is used for poor man's AR instead of using nitric acid for AR. I would say put everything away and stop what you are doing and read then read some more and once you think your ready and understand re read it till it all makes since before you ever start. I am also new to this and it is possible, just read a lot and start off small!!


Tyler


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## cvikatore (Oct 11, 2013)

Thans for warnings, I know that is dangerous but I allready participate some gold with sodium itrate from AR, and the last time something went wrong and I dont know what and I ask for you halp please if you know what hapend to tell me. It is hard for me ro find Smb in my country, my be it will be easier to prticipate with smb? and tell me how to kill nitric some other way instead of cooking?


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## pattt (Oct 11, 2013)

Hi, cvikatore,

Like said before : NaNO3 is NOT a precipitant. Sodium nitrate is the chemical compound with the formula NaNO3. To make your "poormans AR".
If it is difficult to find smb for you, I would give it a try with copperas (iron II sulfate), You can make that yourself if you don't find it. (search, read)

But also, like said before You do need to do much more reading :!: :!: 
All is on this forum, and the book to read (Hoke's) you can download for free (see for the links in the forum)

Do you have stannous chloride ? Do you have a standard gold test solution? (search, read)
What will you do with the wastes?? (search, read)

The more reading you do , the better your questions will be, the more help you will get here.

precipitant, precipitate, but not prticipan, participate.

Pat



I hope you will do everything you do safely, for you and all living things around you :!: 

Pat


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## butcher (Oct 11, 2013)

Chemical names are important, prefixes and suffix in their name is also important.

Sodium metabisulfite Na2S2O5 (we use to precipitate gold), (sometimes new members confuse this with sodium metabisulfate)

Notice the ending in the names, a sulfite SO3 is a different chemical compound than the compound of sulfate SO4, notice the difference in their names ite and ate, these denote the oxidation state or valence, how the chemical reacts, which can make a big difference in their chemistry.

Nitrate NO3, is a different chemical than nitrite NO2.

Sodium nitrate NaNO3 will oxidize gold in an acidic solution.
The Hydrogen from the acid (HCl) can form HNO3 in solution (the principle used in poor-mans aqua regia to dissolve gold).

Sodium nitrite NaNO2 can be used to reduce gold, or precipitate gold from solution, I have never used it or studied its use, so I cannot comment on it further at this point.
Although Hoke discusses it in her book.

Notice these two similar compounds with different suffix in their names, which have different oxidation states, can make a big difference in the chemistry with gold in acidic solutions. 

Names of chemicals are important, this is a major reason we insist on not using texting lingo, and expect users to spell check, that and many do not speak English and rely on translation to read, if we spell it wrong the translation comes out wrong.

Ferrous sulfate, also called copperas (FeSO4 10 H2O) can easily be made with a fairly pure source of Iron (transformer iron laminates are fairly pure soft iron, if you burn off the shellac and wash them), dissolving the iron in a very dilute sulfuric acid (10% H2SO4) will give a green solution of FeSO4, heating this solution to crystallize the bright green copperas will give you a really pure copperas salts, store these ferrous sulfate salts wet with a few drops of H2SO4 acid to keep the crystals fresh, store in them plastic HDPE bottle to keep them from air, (as air can oxidize them to a white-brown salt of iron oxide/hydroxide that will not work to precipitate gold, the copperas is also used to test for gold in a spot plate (a brown ring of precipitated gold around the crystal indicates gold in solution) very useful also when PGM metals are in a gold solution in the test we can remove gold and retest for PGM's (where gold may mask the color reaction of the PGM test).

Study is important, read Hoke's and the forum, the suggestions above by our members, will help you become a better gold refiner, and help to keep you and your neighbors safer.


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## bswartzwelder (Oct 12, 2013)

Butcher,

I worked with transformers for approximately 16 years from 1970 to 1986. I even had the pleasure of designing, building, and winding some transformers. One in particular was for a ham radio friend who needed a transformer with a 120 volt primary and 3 or 4 secondary windings with voltages ranging from 6 volts up to about 500 volts.

The "laminations" for the transformers are made from steel, but have "impurities" added to enhance their magnetic behavior. The names for the two steels are hipersil and hipernik. Both of these are the trade names of Westinghouse Electric Corporation, East Pittsburgh Division, where I worked. Hipersil steel has silicon added to the steel and hipernic has nickel added. Hipernik can be as much as 50% nickel. I don't know how much silicon is added to the hipersil cores, but I do seem to remember they were more common probably because they were cheaper to make. They just weren't quite as good as their nickel counterparts. 

We made "current" transformers for large generators and circuit breakers. The cores were wound on a machine to form a donut shape. Then, they were varnished, wrapped with insulating paper and one copper winding consisting of many turns with current taps at specific points. When testing an entire rack of these transformers, they all had to be short circuited except for the actual one undergoing the testing. As current was applied to a conductor running through the center of the transformers, the output current of the transformer under test would be a direct ratio of the current running through the "one turn" primary conductor. The voltage at the output leads of any transformer not shorted out would skyrocket, trying to approach infinity. Strange how adding something which is basically non-magnetic can enhance the magnetic qualities of steel which is usually magnetic. I say usually, because there are some formulations of stainless steel which are either non magnetic or only very slightly magnetic.


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## butcher (Oct 12, 2013)

bswartzwelder,
Yes of course motors, terroids and transformers can be made out of many different types of materials, shapes and sizes with different operating properties, and many times the core is made to handle the frequency and give to give the desired magnetic flux properties...

Transformers, torroids and motors come in a wide variety of shapes, sizes,, they will also be made for a specific purpose in doing so their construction can vary widely, and they do use different materials to make up the laminate, some transformers use a high nickel iron alloy (similar to stainless steel) some as much as 80% nickel, carbonyl iron, glassy vitreous metals. Ferrite core or donuts, some even add cobalt, as well as other salloys...

These torroid, motor iron or transformers are not what I was discussing making the copperas (ferrous sulfate )from.

The soft iron in most of the transformers is a fairly pure source of iron (it can have from 0 to 3% silicon) and is sometimes referred to silicon steel when the content is at the high end of this range; it is also called electrical steel.

http://en.wikipedia.org/wiki/Electrical_steel

http://en.wikipedia.org/wiki/Magnetic_core

http://en.wikipedia.org/wiki/Silicon_steel

Ferrous sulfate can be made from many different sources of iron, when we crystallize the copperas the iron sulfate crystals reject impurity's, and soft Iron transformer or motor laminates are an fairly pure source of soft Iron, which will make some very nice green copperas crystals, the tiny bit of silicon has given me no troubles (0 to3% silicon seems to be common in the iron laminate), you will most likely have a hard time finding a better or cheaper source of soft pure iron than from transformers or motors to make your copperas from.

And or course we do not want to use a transformer, motor, or torroid that do not use the soft iron laminates.
We do not want to use transformers or motors that use materials like the ferrite core, high nickel, high cobalt iron, Fe-Al alloy or glassy vitreous metal core, powdered magnetic cores or one of the other alloys...

Steel wool, as long is it is not the bronze or stainless steel or soap impregnated should work also (although I have not tried it to make copperas with).

http://go.rockler.com/tech/RTD20000185AA.pdf


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## cvikatore (Oct 13, 2013)

NaNo2 is preciptation sorry my mistake. and I am reading Hook book I see what was wrong nitric was still in the solution but what can I do to whit this mud ? I will boil again the solution that I have without a mud and do steps again but I think that in mud is some gold? 
Thanks for your ansvers


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## cvikatore (Oct 13, 2013)

This is what I got now,


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## cvikatore (Oct 13, 2013)

This is how it looks when it is dry in filter paper, and behind is a glass whit yellow solution that is mud dissolved in HCl acid and there is some gold at the bottom, but it is so tiny particles then when it mix looks like there is nothing and again settle after while.


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## butcher (Oct 13, 2013)

Because I have never used sodium nitrite as a precipitant, I probably will not be much help here.

I would expect the gold to precipitate as a brown powder as it normally does, free nitric acid will normally keep the gold in a oxidized state and keep it from forming a precipitant of the elemental gold brown powders, base metals (my guess is you have several involved here from the CPU's) can also complicate matters, the acids can form salts, such as NaCl as well as other base metal salts, many of which are white or fairly clear crystals, and concentrating a solution these salts will many times form as the water or solution concentrates, these salts could form before all of the excess HNO3 has been driven off by evaporation.

Looking at just NaNO2 and HCl we can see where NaCl common salt is formed as well as nitrous acid in solution:
NaNO2 + HCl --> NaCl + HNO2, 

In most of the reactions where we dissolve gold salts are formed, some methods Like with HCl / NaClO (bleach method, the salts can form in a much larger volume than other processes, base metals also form salts several of which are insoluble or only slightly soluble, especially in a concentrated solution.

Many of these salts can be mixtures of common salts and other metal salts, and can normally be separated, NaCl is water soluble (even in cool water), lead chloride is insoluble in cold water but becomes quite soluble in boiling hot water, silver chloride is insoluble in cold water or boiling hot water, silver chloride can be dissolved in ammonia solution (and precipitated again as AgCl with HCl {read up on the safety of silver ammine solutions to avoid explosive mixtures} before attempting this), copper I chloride will dissolve in HCl ....

With the free nitric and base metals in solution you may have a hard to getting a good gold precipitation, cementing the values out onto copper metal is always an option. 

evaporation may form copious amounts of salts before the free HNO3 is vaporized completely off, here I see several options:
Separate salts to keep solution from bumping or overheating the bottom of the beaker and possibly breaking it due to temperature difference, or scorching the salts to the bottom of the beaker, and deal with the salts formed separately from the concentrated solution, while evaporating the solution to de-nox, (not that good of an option).

Adding a bit of gold to consume HNO3, using heat to drive the reaction to completion.

Using sulfamic acid to remove free HNO3.

Cementing values on copper metal (this is the one I think I would choose, because of the base metals involved).

I have never used NaNO2 to precipitate gold and would like to learn more about it, although I do not have much reason to try it at this point.

I do not know if this will help you any or not, but I can guarantee you Hokes book and understanding what she teaches will help.


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## moose7802 (Oct 13, 2013)

What type of cpu's did you process? Did they have gold caps and did you process the caps along with the rest of the cpu? I remember seeing a post that said when tungsten precipitates it has a yellow orange color. Some of the cpus with gold caps are made of tungsten under the gold plating so maybe that is what this precipitate is? Just a thought 

Tyler


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## butcher (Oct 14, 2013)

The color of the filter looks like it could have an iron salt from the rusty looking color, but the trouble is we cannot use colors as a way to tell what we have, colors are sometimes clues, but can also be deceiving, testing is the only way to tell for sure what you have.

I cannot tell how concentrated the solution is in the large beaker, the dark green solution, it looks to be loaded with base metals.

Then by the filter there looks to be a nice yellow solution, this is closer to the color I would expect for a gold chloride solution (although Iron can give a yellow color also), this is where testing with stannous chloride will help determine if that yellow is gold, ammonium thiocyanate will give a blood red color if iron is in solution, for both of these test it is important to remove free nitric acid before testing, as the free nitric can mess up both of these tests.


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## cvikatore (Oct 14, 2013)

There was 3 intel pro, 4 amd k5, some 486, 286, and some intel pentium... I break it and put all in AR, in first was yellow and after dark yellow brown green, mistake was puting in AR right away I should put first in nitric to remove base metals. I did before with some less Cpus and percitipate some gold but I belive not all from solution and worked with more patience...


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## Palladium (Oct 14, 2013)

moose7802 said:


> What type of cpu's did you process? Did they have gold caps and did you process the caps along with the rest of the cpu? I remember seeing a post that said when tungsten precipitates it has a yellow orange color. Some of the cpus with gold caps are made of tungsten under the gold plating so maybe that is what this precipitate is? Just a thought
> 
> Tyler



WO3 That would be my guess.


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## cvikatore (Oct 18, 2013)

butcher said:


> Because I have never used sodium nitrite as a precipitant, I probably will not be much help here.
> 
> I would expect the gold to precipitate as a brown powder as it normally does, free nitric acid will normally keep the gold in a oxidized state and keep it from forming a precipitant of the elemental gold brown powders, base metals (my guess is you have several involved here from the CPU's) can also complicate matters, the acids can form salts, such as NaCl as well as other base metal salts, many of which are white or fairly clear crystals, and concentrating a solution these salts will many times form as the water or solution concentrates, these salts could form before all of the excess HNO3 has been driven off by evaporation.
> 
> ...




So there is possibility that in AR was more HCl and in reaction with NaNO2 make again HNO3 and that is problem, is there a same problem with sodium metabisulfit because I will get some very soon and try precipitate gold with it. And I made some pictures of salts separated from the rest of the solution. If you know what to do now It will be much of help to me. if put some HCl over the salts it will dissolve and live on the bottom some gold, if will dissolve the gold too?


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## cvikatore (Oct 18, 2013)

salts and the solution that hardly contains some gold.


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## Anonymous (Oct 18, 2013)

How many processors are we talking about here?

If it's only a few then the top picture is likely to be fair representation on the gold you would get.


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## butcher (Oct 18, 2013)

Again we are discussing different chemicals NaNO3 (sodium nitrate) and NaNO2 (sodium nitrite), although both salts of the same acid they act very differently in solution or with acids, even the concentration of the acid and its temperature can play a major role in how these salts react in solution.

Lets look at the nitrate first:
Hydrogen from an acid react with NaNO3 (sodium nitrate) to form nitric acid HNO3 and a salt of the acid used, example: 
H2SO4 + 2NaNO3 --> Na2SO4 + 2HNO3
above we have sodium sulfate and nitric acid (neither of these will dissolve gold).
HCl + NaNO3 --> NaCl + HNO3 (note this one would dissolve gold because of the chlorides involved similar to the SSN leach, and especially if more HCl was used, making a poor mans aqua regia).


Sodium nitrite with cold dilute acid (from the hydrogen of the acid involved) will form Nitrous acid HNO2 (a light blue solution)in solution with acid or hydrogen from the acid, but only if cold and the acid is dilute, this HNO2 is only found in solution,it is also very unstable, and will quickly decompose.
2NaNO2 + dilute H2SO4 --> HNO2 + Na2SO4
HNO2 decomposes in solution to nitric oxide, nitrogen dioxide and water:
2HNO2 --> NO2 + NO + H2O
note this will give a brown gas of NO2 as the NO mixes with the air above the vessel:
2NO + O2 --> NO2 (g)
The NO2 can combine with water in the dilute solution forming Nitric acid and more nitrous acid:
2NO2 + H2O --> 2HNO3 + HNO2
In warm or concentrated acid or solutions the reaction produces nitric acid, nitric oxide and water:
3HNO3 --> HNO3 + 2NO + H2O

sodium metabisulfite will not make nitric acid in solution.

The orange salts look strange to me I still suspect iron (but I could be wrong) the color could come from a number of metal salts.

If you heat a sample of these salts strongly do you see a brown gas evolve? like NO and NO2?

if so I would probably try an incineration, because gold powders incinerated with chlorides is volatile, I would wash powders in a solution of NaOH and wash out the salt formed well with water before trying to incinerate the dried powders to remove the previous acid,and form metal oxides of the base metals involved, then wash the powders with boiling water, , (they will contain base metals, a boiling wash in HCl should dissolve the base metal oxides, helping you to remove the majority of them before you dissolve the gold again, to try to recover gold from them again.

Did you test the solution with stannous chloride or a ferrous sulfate crystal in a spot plate, to see if solution contained gold?
if you suspect nitric is involve a little sulfamic acid added to the test solution in the spot plate, and retry the test again, (GSP has been talking about diluting the solution with free nitric before retrying the test, I have not experimented with it but I believe what he has suggested).

If there is any gold was still in the solution it should cement out of solution using copper, a brown powder would form with the copper if gold was still in solution.

Sorry I cannot help more with precipitating gold using NaNO2, I never tried it and have read just a little about it, I do not think it is popular as I have not seen that much about it.

SMB will precipitate gold from solution, ferrous sulfate also called copperas will also work well and can be made at home with iron ( not steel) and dilute H2SO4 (if you are curious how to make it I have made posts of how I make mine).


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## cvikatore (Oct 18, 2013)

butcher said:


> if so I would probably try an incineration, because gold powders incinerated with chlorides is volatile, I would wash powders in a solution of NaOH and wash out the salt formed well with water before trying to incinerate the dried powders to remove the previous acid,and form metal oxides of the base metals involved, then wash the powders with boiling water, , (they will contain base metals, a boiling wash in HCl should dissolve the base metal oxides, helping you to remove the majority of them before you dissolve the gold again, to try to recover gold from them again.



This is what I will try to do with salts,
I tried before when this happen two mounts ago when I first started with AR but I tried to melt it and got dark staff with gold particles inside. 
I tried with some other CPUs again and got some fine gold but not everything from solutions (still keeping the solutions) I stopped adding NaNO2 so it would not form the same salts, now I made the same mistake.
Interesting is that in a first adding of NaNO2 there is a brown fumes second adding no brown fumes and no gold and adding more NaNO2 again brown fumes and brown mud  again like never did it before. 
I successfully recover some gold from jewelry waste about 1,5 grams of waste 0,8g of gold, dissolved in AR boiled 3 times to get of excess of nitric acid (and had a little problem the beaker cracked cause I boiled too much) but put some HCl and water and NaNO2, color changed from yellow to colorless and brown gold was at the bottom of the beaker. 
My be that I use too much acids and less boiling (now afraid of cracking).
I found smb and next is to learn how to use it.


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## cvikatore (Oct 18, 2013)

One more thing the solution it has to be hot when using NaNO2.


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## butcher (Oct 18, 2013)

cvikatore,

May I suggest you work first with a more pure metal, when learning to use the sodium metabisulfite? Working with a more pure solution with fewer problems will give you a better understand of the reactions involved. 

Memory fingers, the gold plated copper edges on computer memory cards are a good source of gold, Close cut the fingers from the cards to avoid tin or solder, the copper is easily dissolved from the gold foils using HCl and 3% hydrogen peroxide, this forms a copper II chloride leach that will dissolve copper, this leach has been misnamed acid peroxide here on the forum, so many people on the forum discuss its use with this name or sometimes they use AP as an abbreviation, once this solution is made an air pump for fish tanks can supply oxygen, this copper II chloride leach is reusable and can be regenerated as long as copper is dissolved (base metals higher in the reactivity series like iron will contaminate the solution and it will not then be reusable to dissolve copper), (Google the reactivity series of metal this study will help you understand recovery and refining better), the copper II solution is light green color, as it dissolves copper and becomes darker brown when saturated with copper I chloride from dissolving copper into solution, as long as you do not overuse H2O2 there is little chance of dissolving gold with this copper leach, when dark brown adding a little HCl and air will put Copper I chloride back into solution as copper II chloride ready to dissolve more copper, Laser Steve's web site has a document that anyone using this leach should study, to learn how to use it properly.

This will give you some gold foils which after washed can be dissolved, I also suggest not using aqua regia to dissolve these foils for this test, aqua regia can be hard to learn how to use, and unless you understand well how to use it, it can be troublesome because of free nitric acid, (after studying the forum for a while you will learn tricks to eliminate this problem, and learn better how to properly use aqua regia (it is not as easy as the internet lead people to believe).

Try using HCl and sodium hypochlorite (common household bleach) to dissolve the foils; chlorine gas is generated by the NaClO (bleach) in the HCl acid, which will dissolve gold, read up on this and do not overuse the bleach, chlorine gas is much easier to remove from the gold chloride solution than free nitric acid is, heating it for a while will drive off free chlorine as a gas, then you can let the gold solution settle till it clears up, decant the pretty yellow gold chloride solution, and filter it, then you can use the SMB to precipitate the gold, use about as much SMB as you have gold, you can dissolve it in hot water, i would add it in portions with stirring and watch for a reaction, when you get enough SMB in solution you will notice brown gold powder forming from the yellow solution, just a little excess of SMB at this point and a good stir, let gold powder settle well, overnight is good, test the solution with the stannous chloride test, if you still have gold in solution a little more SMB will be needed, to precipitate the gold (I would mix up a fresh small batch of SMB if needed), and use the stannous chloride test to avoid using too much SMB, overuse of SMB can reduce copper from solution, and give a false positive in the gold test with stannous chloride (giving a brown reaction instead of the normal purple color of being positive for gold, this false brown reaction may be due to the copper being reduced in the reaction of the test.

Doing a study of the above techniques I suggested above will help you, learn easier how the reaction with SMB works, and it will help you get a better Idea of ways to deal with electronic scrap, and help you more in learning to recover and refine gold remember we do not want to dissolve gold with base metals, tin or solder are always bad in solution and should be avoided, you never want tin and gold dissolved in the same solution doing so is just a good way to lose your gold.

Keep studying Hokes book, it will teach you the basic principle, these are the most important things you can learn, if you understand them, you will understand basically how to recover and refine gold. You will understand how to keep from forming troublesome mixes, and even when you do form them, you will understand how to get back out of the problem.


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## cvikatore (Nov 16, 2013)

cementing with copper create same brown mud, in the mud is gold...


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## moose7802 (Nov 16, 2013)

Take a little of the mud dissolve in AR or HCL/Cl and test with stannous. Should always do a second refine anyways, to achieve fine quality Au. 

Tyler


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## cvikatore (Nov 17, 2013)

Yes I will do that, what about aluminum for cementing?


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## butcher (Nov 17, 2013)

I would avoid aluminum, it gets very messy, and can form a gelatinous compound which can easily trap values, the reaction with acid solutions can be violent as the hydrogen leaves the acid as hydrogen gas.
Aluminum is also harder to deal with in treating the waste solutions.

I would choose copper or zinc depending on the goal.

Copper will only cement the more precious metals from solution.

Zinc is much more reactive and will cement a wide variety of base metals (zinc will also displace hydrogen from acid).


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