# Potassium Iodide-Iodine gold etchant



## pohyh

Hi All

I am new in this forum and I found that the discussion here is very informative.

I am keen to used Iodine: Potassium Iodide (KI3) etchant to recover gold plated computer/PCB part. I was told that it is very effective but I have not seen any discussion forum on this topic.

Can anyone shed some light on this? I am keen to know the advantages versus other technique, for example, toxicity, gold specificity etc.

Thanks and have a nice day 8)


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## maltfoudy

here is some reading on iodine 


http://webpages.charter.net/kwilliams00/bcftp/docs/halides.htm


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## pohyh

Hi Maltfoudy

Thank you very much for your linformation/ink. I will keep you posted on my finding.

Regards


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## jadesource

Maltfoudy as a miner when I first found that site it opened a whole new world of knowledge for me, now I look back and it doesnt seem like much but it shure was good then. He should enjoy that site. Bill


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## goldsilverpro

In Firefox, it's amazing how much easier it is to read red on black, or any dark on dark, if you go Edit/Select All. I don't have IE but I think on some versions you have to select with the cursor.


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## Juan Manuel Arcos Frank

Pohyh:

Iodine and Bromine are good etchants for gold,but why do not you use the processes that are posted here and work well?.

Manuel


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## jadesource

Manual for me when I read about those things i was applying them to gold and PGM ore from mining ,since then I have learned the many problems that arise with halides in those applications and the many other leaching solutions out there . The more i have in my disposal for testing the easier it is to find the proper one for that particular ore body. Bill


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## qst42know

goldsilverpro said:


> In Firefox, it's much easier to read if you go Edit/Select All



That's a good tip GSP! I have a hard time reading red on black text.


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## pohyh

Hi Manuel/Jadesource

Thanks for your comment.

I am involved in surplus management of semiconductor industries in Singapore. I have many opportunity to get various kind of chip, contact, platter, target, shield which normally contain some way or the other PM.

Obviously the used of cynide is efficient as gold etchant but unfortunately we in Singapore has very strick environmental protection issue. Although AR is better but the toxic fume from nitric acid is simply too much for people around us not to report to the Ministry of Environment (your equivalent of EPA in USA).

That is the reason why I am keen on halide as gold etchant. From literature, it seem that it is very specific to PM. Futhermore, the gold can be reduce in acidic environment using thiousulfate as reducing agent followed by reducing silver and pallanium in the alkaline environment using for example hydroxyl amine as the reducer.

As Jadesource say it correctly, they are drawback on the halide etchant. Obviously is the cost consideration as the KI and I are expensive. Although the Iodine can be regenerate easily using hydrogen peroxide, regeneration of KI seem to be challenging. If some how the KI can be regenerate, it should be prefect answer to this issue. Perhelp, Jadesource, can you share with us your experience on halide as the etchant.

Although some member talk about replacing KI with hydriodic acid and resolve the cost issue, the hydrazine (staring material) is difficult to find here. Afterall. I have all the necessary chemical to work on KI3 method and I just want to get around to perfect this method (If I can!).

The question I would like to throw to the forum is that is there any suggestion to regenerate KI. My understanding is that some of the base metal is being dissolve in the KI3 etchant and reduce it efficiency. In addition, any input or experience working on this type of halide etcant will be helpful.

Thanks.


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## Juan Manuel Arcos Frank

Pohyh:

Let us suppose that I tell you how to make cyanide,how to eatch gold with iodine or how to make KI...Would you share freely your process with all the Forum?...Would you keep all the Forum informed about your progress step by step?.I can tell you but I need you to answer the questions above cited.

Regards.
Manuel


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## jamthe3

Wow, c'mon Juan Manuel, given you exchanges on a different thread...this seems like an odd request you're making of the gentleman. If he is the kind that won't, surely he'll answer affirmative anyway to get what he wants; and, if he's the kind that will...the questions are immaterial.

But, as was GSP's...the info is yours to do as you wish. Either way, I always enjoy (and learn from) your posts so hopefully he'll give you the answers you're looking for so I'll benefit from yet another.

Cheers,
John


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## maltfoudy

I posted a link for information that was asked for,the reason he wanted to learn about iodine wasn't an issue.unlike mexico nitric costs alot here and any method that can be regenerated has interest to many. including myself,so if he can take what i gave him and come up with a solution to his problem,maybe he can help me with mine. i would much rather spend 400 once on iodine than 100 ten times for nitric.


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## pohyh

Hi Manuel

Thank for your feedback and your request.

I am really new in this Forum! Please educate me if I am wrong. I thought I am in this Forum where a group of peoples with common interest come and share their experience on, in this case, gold etching or related subject. With the sharing of our experince, we can cut down the time (for not reinventing the wheel ) or save money (using a more efficient technique). It go without saying, when time come, each and every member, I included, has an obligation to put in writting, telling all those who are keen, on our topic of interest (in my case KI3 etcant). 

Anyway, the way you write seems to be a little "hard". Is that the common practise in this Forum? Or it is the way you write? I am a newbie but I took your comment positively.Perhelp the way you put in writting can be refine in the near future
:wink: 

Regards


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## Platdigger

hahaha, sorry about that pohyh. You just missed all of Manuels ranting
in another thread.
I am sure it is nothing personal, just Manuel trying to make a point.

Point taken Manuel.......

Did you do a search of all the posts on this forum about iodine?
There was a real interesting thread, it was titled something like "you won't believe it! Iodine but with a twist".
Anyway, the general consinses was that it was to dangerous for the average joe to even try.
Randy


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## pohyh

Hi Randy

Thank for your comment and indeed you are right, I should have read the comment post by Manuel in the other thread before responding to himl! Anyway as I said, I took the his comment positively and Manuel definately have a pont and he put the strong message right across, I hope, not only to me but to every single member of this Forum.

I studied analytical chemistry and specialised in chromatograhy before going on my own probably 10 years ago to be a surplus management agent for semiconductor industries in Singapore. With that information in mind, I hope you do not have to worry for me on handling of iodine. 8) 

Anyway, still look for information on experience on people/member who have work on iodine as etchant. Any infor should be a ++ for me.

Regards
Poh


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## Juan Manuel Arcos Frank

Pohyh:

OK,let us do it.Please,chech out if you can get the following,there,in Singapur:

-KI Potassium Iodide
-I2 Iodine metallic
-NH2OH Hydroxylamine
-NaOH Sodium Hydroxide
-H2O2 Hydrogen peroxide (30%)
-Distilled water

The process consists in making a solution of KI and I2 which dissolves the gold layer of e scrap forming soluble complex of K,I and Au then a reductant is added,the gold precipitates and the solution is regenerated.

If you can not get any substance of the list,please,tell me.It would be desirable that you take a look to Steve´s videos about gold contents in e scrap.What kind of scrap do you have?.The process needs 500 gr.,at least,of cutted fingers or gold plated pins or ceramic CPU chips.

Pohyh,I offer you an apology,my english is not good enough and sometimes I think in Spanish trying to write in English.I did not seem too hard.If you are willing to recover gold with KI/I2 I am willing to help you.

Regards
Manuel


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## Juan Manuel Arcos Frank

jamthe3:

I do think that Pohyh has experience in Chemistry,since he wrote KI3 (instead of KI)...KI means Potassium Iodide...KI3 is the complex formed with gold in this process...Let us try.

Regards
Manuel


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## goldsilverpro

http://www.google.com/patents?id=oLZ7AAAAEBAJ&printsec=abstract&zoom=4&dq=3957505

I think this patent contains all the chemicals you mentioned and is the source of that method. Go to the EXAMPLE near the end - it tells exactly how to do it.


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## jamthe3

Juan,

I wasn't the one talking about the experience or dangers...Heck, I'm scared enough of my own shadow...LOL!!

I was the one teasing you about the requirements for your sharing how to do it; and believe me, that's all it was, good natured teasing.

Estoy poquito tonto y necesito apprender mucho mas....en como hacer oro y como hablar espanol tambien!!!

Salud,
John


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## pohyh

Dear Manuel

First of all, thanks for your input and sorry for misunderstanding you on the message you try to put across. Not hard feeling, I take your point positively.

I have got some KI, I, KOH, NH2OH (+dioniser water) from the local supplier. My intention is to play around with ratio of KI:I:H20. I will fixed the I to 1 and H2O to 10 and probably try to vary the ratio of KI from 3 to 6. 

Subsequently I will drop a piece of preweighed gold (99.9 around) to a 50 ml of the various ratio of KI3 etchant. When the colour of the KI3 etcant change colour to colourless, I will tke out the gold and weighed them. With that I can find the optimal KI3 etchant rotio.

Obviously the percentage recovery of gold with hydroxylamine (I think I will start with 30% weight: Weight with H20, pH to 8 and buffer with K2PO4) can be determine easily since I know the weight of gold in the KI3 solution.

The 2nd parametr should be the temperature (35 C to 60 C?) may be a good try and least but not last, perhelp ultrasonic sonication may be incoporate later.

Can you comment on the above? 

Regards
Poh


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## Juan Manuel Arcos Frank

John:

You speak spanish pretty good!!!!!....Would you be my teacher?...look...what does it mean BTW?.

Behave yourself.

Manuel


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## goldsilverpro

BTW. By the way,.....


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## Juan Manuel Arcos Frank

GSP,my Dear Friend:

Yes Sir,this patent works with this method.It has the disvantage of cost,because is more expensive than AP&Clorox methods.The good news is that works lovely with gold refractary ores.

Have a nice day.

Your friend
Manuel


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## Juan Manuel Arcos Frank

Thanks,GSP...


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## Juan Manuel Arcos Frank

Pohyh:

Read the patent that GSP has posted...here is the method,Iodine will be release,be careful.

Regards

Manuel


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## DNIndustry

I was the one who starting posting about this.
both KI/I2 and NH4I/I2. So far I have 6LB's of I2 I can reuse. 
The NH4I/I2 is much cheaper and rate controlled. 

Both ways work. Same idea as HCL + CL

I am not going to say any thing negative about the methods suggested in this forum. They work, very well...

I doing so I am trying to show respect. Something I dont that is given to alternate ideas. ( I do mean this peacefully)

I tried to get answers and got criticism. I had to figure it out completely on my own, but I did.
Never had any "bad" reactions
I got results. It works. 
I decided I wasnt going to make waves....so I havnt posted anything further about it.

If you need help PM me I dont want this causing an uprising. If others want to know Ill respond openly..Ill let the forum decide.
-DNIndustry


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## lazersteve

DNI,

I for one am very interested in the Iodine processes. I would like to see your findings posted to the forum.

A few years back I did a little testing with iodine but was not fond of handling the iodine as it's a little messy in my opinion. I also had problems separating and identifying the precipitated gold. A bigger drawback to the iodine methods are that iodine and it's compounds are one of the most watched chemicals by the Feds in America due to their use by illicit drug manufacturers. 

On the plus side the reaction was more selective to gold and worked quickly.

Hydrochloric acid, 3% Hydrogen peroxide, and Clorox bleach are very common chemicals and that's a big plus for me. They may be slower, but since I'm a small refiner, time is not critical for me. All the gold that I refine is either for a few select customers or put away as a long term retirement plan.

Steve


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## jamthe3

I would love to read about it as I'm sure Pohyh would also, seeing as he started the thread.

Juan, thanks for lying about my spanish fluency. I now feel like walking across the bridge, chest out, full of bi-lingual courage, ready to......look in my translation dictionary first time someone asks me a questiong not in the "present" tense.

BTW stands for "by the way"

Cheers,
John


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## Platdigger

Same here DNI, I would be very interested in what you found out about this proccess.

Think there may be any special dangers doing this with gold bearing ores?
Randy


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## pohyh

Hi DNI

Obviously I am seriously keen on your experience on halide etching and I have PM you on my request.

I for one believe in sharing my experience I have on the topic which I am keen on. Sometime I got positive and sometime negative comment. Nevertheless, all input is taken positively. You are talking on creating a wave on your finding, who know, your wave might have a chain reaction and turn out to be tsunami for us in gold etching process!

I remember when Einstein put up his E=MC2 equation, for him is wave, but subsequently input from various other scientist made it a world greatest physic equation!

Keep up your good work!

Regards
Poh


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## usernameguy

I've turned on to this recently. I simply add enough KOH to the Iodine etch solution until it turns clear (well, cloudy, then clear after settling). M precipitate has typically been a greyish color. The solution is discarded, so I figured I might as well recovery the Au. All I've really found is we're "dumping" the solution well before it needs to be replaced as 1gal will dissolve 100g Au. I suspect the reason is because the etch rate will start to decrease. We're basing our process on about 30 Angstroms per second. If anyone has any eperience on the linearity of the etch rate with Au saturation, I'd be interested. For now, I'll let em do what they're doing till I know better. It's kind of too bad, I just discovered this practice, and have only done it once, recovering about 15g of precipitate from a gallon of solution. All I care about for now is if this is pure gold, and am curious whether the etch rate is linear to saturation. I doubt it just using simple reasoning and a basic chem knowledge.
Guy


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## Juan Manuel Arcos Frank

I completley agree with Steve,AP & Clorox methods are the best,they are cheap,all substances are available in the supermarket and both processes have proven to work well.The problem is AR,some countries limit the use of substances,especially acids,sometimes poor`s man AR solves the problem.The problem of toxic fumes remains unresolved.
This is precisely the task we have to do,find and investigate new processes,some will work,others will not.

To prove what I just said I am going to post some information about Iodine Processes in gold ores,I hope this helps the Forum`s Members to investigate and experiment with these processes in the gold scrap recovery field.

I wish you all a nice day.

Manuel


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## Juan Manuel Arcos Frank

Guys:

I am such an idiot!!!!!!!!!...Would you tell me how to post al these files together?....BTW...Would you tell me how to quote?.

I do appreciate

Manuel


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## Juan Manuel Arcos Frank

here the last one


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## Harold_V

Juan Manuel Arcos Frank said:


> Would you tell me how to post al these files together?


Unless there are unusual circumstances, all you need do is add them one at a time by clicking the attachment button. Do be aware that the first one in becomes the last one viewed, so if you have something that is best viewed in sequence, post them in reverse, last one posted will be on top, with the first one posted on the bottom. 



> BTW...Would you tell me how to quote?.


Simple:


Code:


 On your keyboard, enter  [quote] Then enter your message, and close with [/quote]

Note that you *do NOT *click the code button. That has been clicked so the needed code is displayed.

If you want to make reference to the source that is quoted, you would enter it thus:



Code:


[quote="Harold_V"], enter your message, and close with [/quote]


By *not* clicking the code button, the above would appear this way:


Harold_V said:


> enter your message, and close with



Hope this helps.

Harold


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## pohyh

Hi Manuel

Thank you very much for your input on the above mentioned subject.

When I studied for my master degree in analytical chemistry in a UK university, my mentor professor used to give me lot and lot of useful information for my study (BTW my field of experty is chromatography, ie seperation technique). When I start work, I missed my good old day in University until I come to this Forum.

To you and all the member of this Forum, I will put up a "thesis" once I have any concrete result on this topic!

On another issue, I totally agree with you on the problem with AR. Here in Singapore, toxic fume, be it generate from HCL or H2NO3, it unaceptable with the local autority, unless you have a proper ventilation to clear your gases. You need to apply for a proper permit with local Environment office and by the time they give you a permit, you must have lost your interest on gold recovery! Doing it secretly is out of the question as SIngapore is a small urbanised city. Just for ilustration, a car drive at 80KM /hr from East to West or North to South will be less than a hours!

Again thank for your input.

Regards
Poh


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## goldsilverpro

I went to Singapore, buying electronics gold scrap from manfacturers, about 10 times in the mid 70s. It was a very strict country. Throwing out a cigarette butt could cost a several hundred US dollar fine. Men with long hair had to get a haircut at the airport before they could enter the country. However, it was the cleanest city I'd been in (the Paris of Asia) and the wages were about 10 times more than the rest of Asia. I loved it there, after I got a haircut.


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## Platdigger

Say usernameguy, can you tell us more about the iodine proccess you are using?

Is this done at a company that you work for?
Randy


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## Harold_V

goldsilverpro said:


> after I got a haircut.



You with long hair? Really? I figured you for a conformist type. 

Harold


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## pohyh

Hi GSP

I thought I am speaking with a young man but by the way you write, look like you are a good old wise man well verse in your field! 

Yes you are right, at 70, the house rules are very strick and go without saying, that was a "fine" country, ie you get fine for every single mistake you commit. Well, I am fortunate as I was still a young teenage running around! 

Obviously things change nowaday. We are going to have 2 casinos very soon (2012?) and FYI there is no more barber shop for long hair's guy in the port of immigration. You can come in with short hair, long hair or bald ie no hair!

So much so with SIngapore...now a little update on my study. Manuel just pass me some interesting on alcoholic halide gold etching. I have read them and look promising. I have also conduct some priliminary study on AP etchning versus Halide itching. What I can say now is that halide work well in sample that is expose (eg gold pin) while as AP is really economical and it work really well, as Steve suggest. The advantage of halide etch is the time. 

Anyway, my concern is still the environment issue. I will persue the halide issue and come out with a recepie in due course. Perhelp, I will look into way and mean to address the environment issue with AP later.

Regards
Poh


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## Juan Manuel Arcos Frank

Harold_V:

Thank you very much!!!!...I do appreciate all what you have done for me.Now I know how to quote.

Have a nice day.

Manuel


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## Juan Manuel Arcos Frank

Pohyh:

This is what de Forum is for.Here is the cherry pie.

Regards.

Manuel


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## pohyh

Dearl All

While woking for my project, I realised that the tap water I used for AP project seem to be "etching" my gold away. Futher investigation reveal that the residual Cl2 in the water might be responsible for this process.

I do not want to spend money on DI water and thus I used condensed water from my airconditional unit and now the problem have been solved. A checked with the resistivity meter indicate that the resistance of commercially availble DI water and the condense water is the same.

So save money by using recycle condense water for your gold recovery.

Cheer! :wink: 

Poh


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## DNIndustry

Sorry Ive been away... Been prototypin.

I guess a back story, Ill also have to dig up my notes later so if I miss something just ask.

I attached the 2 patents that have been mentioned. The first is the KI & Iodine. The second is NH4I/I2

Comparatively using potassium iodide is much more costly than ammonium Iodide. The Problem is that the KI concentrations shift up and down. Always having a fresh batch mixed is much more desirable. The other draw back of KI is the acidic nature. PH is 2-3 ish if recall. Because of this the etching rates are much less controllable. If it is left in too long it will chew right into the nickel substrate and the copper below. ( If on pins)
The PH of NH4I is 7.5-8.5. slightly basic and much more selective.
I would generally do the etching at 40-50C ish. It can be done in a container in a waterbath, crockpot to cheepsk8s  
Fume wise a hood is not needed, if you do it properly. A mask is recommended for some portions (initial mixing, precipitating the Iodine back out.)
The nice part about experimenting with KI thought is the amount of elemental Iodine you can accumulate. - 

A 500g Container of KI yields about 3 mols of KI-
K=39
I=127
KI=166
Of the overall mass there is 382.5g elemental Iodine/500g KI

I may have said this previously but I am easily pushing 6lbs of Iodine. It is cumulative, any reuses. The potassium is lost to the gold gods.

So you can atleast see the cost difference, 
it takes about 450g I2 & 97mL's NH4OH & 47 mLs 30%H2O2 (make sure I dont have these numbers switched)
Comparatively the ammonia is much cheaper, and controllable

* Before I get flamed, A public service anouncement, make sure you add the H202 exacty like and when it says*  That one little oxygen molecule is what prevents making the bad stuff. 


In this case more is not better,
H202-Make certain that you are using 30% not 35%. If so properly dilute your solution. Stir excessily well. If you follow the patent 
Add 500mLs Water to a 2 liter reactor
Add 350g I2 crystals & stir
-----
The iodine is not soluble in water. Infact one time I spilled half a pound on the floor. Scraped it up, rinsed it, tossed it back in. Not even a slight stain.
-----
Add the H202
-----
This makes the Iodine soluble
-----
Add the NH4OH- Use a mask it is harsh, add slowly in increments and keep the stirring up.
-----
I took a 5 gallon bucket, cut a hole in the lid. Put a bearing in the middle and mounted a paint vortexer, put my drill on the other end and bam, best $3 I ever spent. 
H202 oxidizes the Iodine, If you read further it talks about adding 3% h2o2 to the bottom of the mixture during stripping, and 30% during regeneration. 
Im jumping ahead but the mixture is actually a 2 level suspension; not really visibly noticable. The NH4I etchs the gold/pt/pd/Ag etc, Then Iodine binds with it. Small amounts of h202 will free up more iodine thefore speeding it up.
* A note of caution if you do this, do not add it near the pieces being etched. It will seriously speed up; Ive stripped parts and only puting the 3% kicker by one of the pieces. All the parts came out looking like brand new nickel plate...minus the one with the hole in it down to through the copper 
*Agitaion is a huge help, remember it becomes a suspension.
Now that I think about it, when I used KI the results even in batch varied (amount etched) The NH4I everything is uniform and bright n shiny. I know Ive posted pictures before.. pH is important, less acidic, less basemetal etching.
Which reminds me...Ive been building this rube goldberg reactor/ion exchange column, after alpha testing my AP, HCL-CL, Resin load/elute process. I am going to try AP, KI/I, Resiload elute on my foils. The best of both worlds. Copper is gone, KI/I will eat it in under 3 mins, then load it onto the XAD-7, elute with acetone+hcl. 
Heck, I wonder how well HI+H202 would work for base metals 
Digest it with HI/I
Load....
Talk about fast an pure, HCL-CL & XAD7 without disolving basemetals yields 99.96% with alluvial ore, imaging feeding it clean gold...

I will continue this later, post questions, comments, Ill answer.
In the mean time 
*Do not try the "make it more basic precipitation theory for gold"
*Do not use hydroxylamine hcl unitl I can get into the use of DiBasic Ammonium Phosphate buffers.
*Do add more H202 when mixing if it still smells like ammonia after a few minutes of beating it with a pail mixer

-DNI


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## pohyh

Hi All

This is the first time trying to post a picture in this Forum. Thank Steve for his tutorial and let see what do we have in Singapore. This are typical precious metal containg sample we get from semiconductor industries.

I am posting 4 pic today and I just post one by one. To play safe!

Regards
Poh

[img:648:486]http://img519.imageshack.us/img519/2384/miscgoldplatedpins.png[/img]


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## pohyh

Dear All

Another pic.

BTW Anybody have any working experience on this HP Injet printer head contact?

Regards
Poh

[img:648:486]http://img259.imageshack.us/img259/6942/hpinjetprinterheadconta.png[/img]


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## pohyh

Dear All

3rd picture. 

[img:648:486]http://img259.imageshack.us/img259/8995/probercontactpins.png[/img]


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## pohyh

Dear All

Last picture for today!

Have a nice day!

Regards
Poh

[img:648:486]http://img17.imageshack.us/img17/21/semiconductorplasmaring.png[/img]


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## usernameguy

Hey Randy, et al.

Thanks for asking. I'm new to all this stuff on the refining end, so still learning terms and such. sorry for the delayed response, family is ill right now. To answer you question, I work in a semiconductor processing facility, so I'm sure I can be of some use if you all are having issues at times. 
my process is relatively simple. The I etchant is used by the facility to etch thin films of Au to create layers of patterns from the wafer (Si) up. The Au that's either plasma sputtered or evaporated then gets covered with a photodefinable polymer and developed away where it's been exposed is 4 9's pure. 99.9999!!!! The Au that's now exposed where the polymer was dveloped away gets etched in this I solution. It's purchased from a chemical supply company, and thrown away as waste WELL before it's saturated. I'm just curious if what I'm dropping out with pure crystaline KOH is pure Au or not. It's doubtful there's much Pt, but possible. The thing is I'm getting a grey precipitate and there's no way to know how much I should be getting. I'm also secondarily curious if the etch rate for the people processing is linear or not, because if it is, I could convince them to not dispose of the soltion so quickly, and this would mean less waste, and less material for me to deal with also. lemme know what anyone thinks, or if you have any questions. 
Thank you in advance!
The other waste solution I have access to is a Au plating solution BDT 510 I believe that again is commercially available. It was recommended to precip this using H2SO4, and I'll be trying that this weekend.
-Guy


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## goldsilverpro

99.9999 is SIX nines. Count them.

Please let us know how the 10% H2SO4 works on the BDT 510. I would try a small sample at first.


Pohyh,
Too bad you can't use cyanide. Everything in the photos would fit it perfectly.


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## pohyh

Hi GSP

I know very well cynide is the most effective interm in etching as well as cost....BUT, we are in Singapore. Although we can buy cynide (we have licence to do so) but to do it is really pain in the neck!

Firstly Environment officer will inspect the storage facility. They will ask tons of questions on the intention. They will check on daily usage. They will do a surprise check on your stock and so on and on!

With those kind of harrasment, I think I would rather forget on using them. Afterall, the disposable issue is very costly for cynide in Singapore. 

After giving you all the excuse, I must admit, the most important fobia I have is that one of my supervisor commit suicide with cynide (way back in early 80) and I am always shy away from it. Afteall, I am such a clumsy guy that I am not surprise if pour acid into the cynide solution one of this day.
 

Anyway, any suggestion on the HP Injet printer head contact. KI3 seem ineffective as the gold is sandwitch inbetween 2 layer of polymer.

Regards
Poh


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## goldsilverpro

Incineration?


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## usernameguy

Our metals guy always refers to the # of 9's as how many are behid the decimal since the 2 in front of the decimal is inferred. Maybe that's just his own personal way of doing it. 
Anyway, Pohyh, Parylene is a very common polymer used to protect electronics, however I think it's mainly used for biomedical devices since it's one of the more biocompatable materials that can be evaporated uniformly, so this may be worth a try. I can ask what's used to remove this, but I'm sure it's not easy. Alot of the polymers that are solvent resistant after curing are an endless pain in the arse to tool engineers like myself because they're so hard to remove. sometimes, they end up rendering $100K tools useless because hot HF isn't an option in the areas these materials accumulate on the equipment. I'd google parylene and see what's mentioned for removal. Even if your material isn't exactly parylene, I suspect whatever can remove it can remove that. As the pro said though, burning it would be simple, cheap and effective. I don't imagine you need to protect any of the other materials involved.
-Guy


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## goldsilverpro

> Our metals guy always refers to the # of 9's as how many are behid the decimal since the 2 in front of the decimal is inferred. Maybe that's just his own personal way of doing it.



Your metals guy is wrong. Colloidal silver people make the same mistake when they talk about pure silver wire. They're wrong, also.

I guess that one can count the 9s anyway they want to. However, universally, in the PM trade, all the 9s are counted, including the two on the left of the decimal point. Counting the 9s in a different way will just create confusion. 

At one time, I was considering selling 4-9s (99.99%) wire to people that made their own colloidal silver. There was about an 800% profit in it. Some sellers were selling 3-9s and 4-9s wire and were saying it was 99.999% and 99.9999% pure, respectively. Anyone that has a grasp of metal purities would know that that was BS. I don't think these sellers were making these ridiculous claims fraudulently. I think they were making them out of shear ignorance. To me, though, it certainly confused the issue.


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## pohyh

Hi GSP

I thought of incineration as well. But when I incinerate them at 800 C, I cannot get any gold. Perhelp the gold layer is thin or Au evaporate in that temperature. 

Any comment?

Regards
Poh


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## Harold_V

pohyh said:


> I thought of incineration as well. But when I incinerate them at 800 C, I cannot get any gold. Perhelp the gold layer is thin or Au evaporate in that temperature.


I'm jumping in this thing without knowing the facts, so please bear with me if I am screwed up. Please set me straight if so.

If you have something that is gold plated and it seems to lose the gold in incineration, rest assured, it has not been evaporated. Gold has the ability to migrate into other metals, although not all. It is for that reason they plate nickel on copper based alloys before applying gold. I expect that if you incinerate, and can't see the gold, it is still very much present, just disseminated in the substrate. Dissolving the base material is likely to yield the seemingly lost gold. 

Harold


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## goldsilverpro

At that temperature, there would be no evaporation of the gold. I would imagine that, while burning off the plastic, there could be enough turbulence to send the light ash containing the gold into the air. I still think that some sort of controlled incineration would collect the gold. Don't ask me how. It's something one must play with. It's a difficult item. Do you have any feel for the amount of gold in that material?


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## DNIndustry

Can some one quick throw up the balanced equation for Au NaClO HCL
Im reading through some documentation, and I know this guy is smoking crack....

Just out of curiosity how does nickel respond to HCL+CL.


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## pohyh

Hi GSP

You might be right. I will try to extract the base metal attached to the crucible and let see wheather I can find any of my lost gold. Incidently some one told me that if I use a zicromium crubile with lid, I mght solve the problem. BTW anybody have that experience?

FYI, Harold_V, the gold content is approx 1 to 2%.

Regards
Poh


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## lazersteve

DNIndustry said:


> Can some one quick throw up the balanced equation for Au NaClO HCL


This primary reaction can be considered the reaction of Cl2 with HCl:

2Au + 3Cl2 + 2HCl --> 2HAuCl4 

The Chlorine is generated _in situ_ via the reaction of the sodium hypochlorite with the HCl.



DNIndustry said:


> Just out of curiosity how does nickel respond to HCL+CL.


 It dissolves.

Steve


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## Juan Manuel Arcos Frank

Pohyh:

I am working with PM recovery from printing scrap(i.e. fil circuits of ink cartridges like you have posted) and I can not be able to get a measurable quantity of gold from 200 film circuits,of course,my scale just can weight 0.1 gr.

The little circles in the film circuit are gold plated,there are very thin wires inside the film circuit ,I do not know if they are gold or copper,since I got a poor quantity of gold I sent them away,I despair with ease.

I hope post my research results soon.

Regards

Manuel


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## pohyh

Hi Manuel

Thanks for your input.

The top layer can be remove by the addition of tetrachloroethane (TCE). After socking the layer with TCE, the polymer basically peer off and float to the top. The small round gold plated disc as well as fine wire drop to the bottom. I strongly believe all those are gold plated.

After saying that, I must say that NOT all the printer head contact is gold plated. I have collected quite a few different type, for other brand of printer are not gold plated. The colour of the disc is slightly brownish.

TCE is good solvent but it does not smell too nice. Just for your information. That is why I am looking for other better technique.

Regards
Poh


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## Juan Manuel Arcos Frank

Hi Poh:

Thanks for your information.Have you tested the small wires for gold?.They seem to be copper.

Regards.

Manuel


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## usernameguy

In the semiconductor industry (at least our research facility) the most common metal deposited before Au is Ti. This is used as an adhesion layer since A doesn't adhere well to Si, SiO2 and a lot of various other materials. the adhesion layer is typically Very Thin respectively. On the order of 50 Angstroms (5nm) (the distance you fingernail grows in 5 seconds). The Au is then however thick the process requires (typically less than or right around a micron. These films are still so thin, they float around in solvent before settling, like gold leaf.

I have a kind of unrelated question. I'm going to precip my Au plating solution today as suggested by GSP, but the last time I filtered off my Au powder precip'd from the I etch solution, I tried to burn off the paper filter using a normal butane torch like that used to solder pipes. It smoked something fierce, and had a very dark smoke. I surmised I was starting to burn off the Au. Any ideas, and is my assumption even possible?

Thx,
Guy


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## AuMINIMayhem

TCE.. that should come with a very large warning sign.. :wink: it's brutal stuff.

I too looked into print heads at one point... there's one of those "Cartridge World" type places near me that junks all the old printer cartridges they have no use for.. the print heads (especialy HP model inkjets) do "look" like they have quite a bit of gold, but indeed angstroms is the key word.. they are nowhere near HGP (heavy gold plate) it's just enough to keep them from corroding from the ink.. which is another problem altogether.. I really thought better of dealing with print cartridges the first time I tinkered around with one.. injket ink not only stains it STAINS! The ink is formulated on such a small scale (nm) that the particles will damn near tatoo you just by contact.. the particles are indeed small enough to absorb instantly and become a sub-dermal stain that takes quite some time to get rid of (Ie: you'll have to wait to shed those cells).. not to mention clothes, etc.. wasn't worth harvesting, IMHO, but I'd be interested in yield data for sure :wink:


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## goldsilverpro

You won't evaporate metallic gold. It can be mechanically carried off in the smoke, especially with a lot of turbulence. You must have a lot of other stuff combined with the gold. However, if you don't like the smoke, can't you leach the gold from the precipitate with AR or, maybe, one of Steve's methods? You're going to need to purify it eventually, anyway.


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## pohyh

HI GSP

I have tried the AP method as suggested by Steve. Initially, some of the gold plated disc came out but disappear (probably the cu portion being dissolved), but most of them stick to the plastic. All of the fine wired remained there. 

As mentioned previously, the metal are being sandwiched in between 2 layer of plastic. As long as I can get to etch one of them, I should get the problem solved. One of the study is obviously suing the chlorinated solvent eg Tetrahydrofuran (THF) or Trichloroethylene (Chloroform) or Tetrachloroethane (TCE). All these 3 solvents work but they stink and all of them are not environment friendly. As mentioned by AuMINIMayhem, TCE is BRUTAL!

Anyway AuMINIMayhem, Hewlett Packard has a IJMS (Injet Manufacturing) facility in SIngapore. Thanks goodness, all the contact we get are production scrap and not from individual injet printer head. You are right, it is pain to work with used injet. The ink simply stain!

On the other subject, usernameguy suggested the sandwich layer might be parylene. Obviously knowing that HP Singapore do not use parylene in their process simply eliminate parylene as the sandwich polymer.

Hi Manuel, previously we have do an etch method via dilute nitric acid and followed by AR and confirmed that it is gold and by wt/wt basis, it range from 1 to 2 %. There are such a big variation depending on which portion you test. Gold plated dics portion higher compare with fine wire portion.

Thanks all for yours input and all your suggestion made this discussion lively. Keep it up.

Regards
Poh


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## usernameguy

Can Au be evaporated in vacuum? The process they use in my lab they "call" evaporation, but... The vacuum has to be very low (or high depending on how you look at it. technically high)in this case Ultra high vacuum. The gold which is extremely pure, as stated 4 9's or better is heated with an electron beam (electricity) focused and directed with magnetic fields. The material Au, Pt, Al, whatever then coats everywhere in the chamber, but mostly up which is where the substrates are mounted on a spinning carousel a specific distance from the source in order to achieve a uniform continuous film. I'm just curious if you guys think this is truley evaporation. I know this is a far cry from a butane torch at atmosphere, but...
I'll start another thread if this is of interest. I don't want to hijack this one. I too am learning much and using a similar process. I think the Au I precipitate from the Iodine solution using KOH is pure though from the patent I got the process from.
by the way, that's actually true about the fingernails. pretty cool huh? We image things on this scale(beyond the physical limits of optical microscopy... visible light's wavelength is way too big). If the temperature of the sample is different than that of the chamber, you end up chasing the thing around you want to see. sorry, I'm kind of a lab geek and new to forums. I've noticed people usually keep ther comments short.
-Guy


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## pohyh

Hi Guy

The term "evaporate" I used is refer to a suggestion that gold "disappear" in the surrounding environment during heating and not the physical evaoporation of pur gold as we have studied in our science lesson. Looking at the physical properties of gold inself, the melting temp is already high, the evaporation is difficult to attain in the normal environment.

Anyway, the picture I post simply mean to tell the member of Forum what I have been working with. I really appreciate the input from the member on the way to remove the gold from the injet printer contact head.

Anyway, I started this tread is on the halide etching. I am here to follow up a bit what I have learn from the process. 

For the KI3 etching, to recover KI in the spend etching solution is out of the question as KI gone to the gold's god, as one of the member put it. Nevertheless, to reconever Iodine from it is a simple task (by adding H2O2). To made the process economical (as KI is expensive, approx US$70/kg), I though if I2 can change to KI in the folllowing equation:

I2 + 2KOH (aq) --2KI + H2O + H+

It is a wild idea right from my crazy mind. Just to see any suggestion from the Forum member.

Any comment?

By the way, DNI has suggested using Ammonia solution in replace of KI. It definately solve the economical issue (Ammonia solution 21% only cost US$0.8/kg) and it work pretty neat. Off course, you must work in the fume hook or well ventilated enviroment or your neighbour will come after you...real fast! :lol: 

Regards
Poh


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## Juan Manuel Arcos Frank

Poh:

Be careful with the wild ideas from your crazy mind.....they can become reality!!!!!!!.

You can make KI like you said,you just need an old trick,here it is:

You have to add some organic acid to the mixure and probably heat a little.If you add iodine to potassium hydroxide this will happen:

3I2+6KOH=5KI+KIO3+3H2O

you will make potassium iodide,but you will get undesairable potassium iodate too...so the trick is adding some formic acid wich will react with the potassium iodate and will form pure potassium iodide,a lovely process,does not it?

KIO3+3HCOOH=KI+3H2O+3CO2

Do you want to know more about this process,let it be:

Mix 1270 gr of iodine(5 mol) with 560 gr (10 mol)(dissolved in 2.5lt) and heat a little bit to complete the dissolution,the iodide and iodate mixure is formed,then heat and slowly add 230 gr (5 mol) of(100%) formic acid ,you will see some fumes and a decolorization will ocurr and you will get a pure solution of KI.

Poh,I welcome you like to experiment...I know you have some H2O2 (30%) in your lab...Would you do for me an experiment?

Regards.

Manuel


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## pohyh

Hi Manuel

My gut feeling tell me my crazy idea might be reality as the synthesis of KI is via formate path (ie addition of formic acid) but I am simply refuse to accept it. Obviously, I want to try and if what you say is achiveable, then we can come out with an economical way to etch gold.

As the Singapore Rule on H2O2 is concerned, we can buy H2O2 as long as it is less than 20% concentration. SO I have plenty of 19% H2O2. I am more than willing to try the H2O2 experiement for you if I can do it with that concentration. PM me if you want that discussion to be private.

Again thanks for your input!

Regards
Poh


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## pohyh

Hi All

Just an update on my recent finding on recovery of precious metal from the sandwich layer of Hewlett Packard Injet printer head contact.

Basically this sandwich layer must be removed before the gold plated metal can be removed. After a series of experiement, I found the the following procedure work pretty cool.

1. Soak the above printer head contact with 50% H2SO4 
2. add 1 part of H2O2 (~20%) to 5 part of diluted H2SO4
3. Shake it gently
4. A few minute later, you basically see the sadwich polymer "charred" and float to the top
5. If necessary, add more H2O2 until all the sandwich layer is being removed.
6. Now you are ready for the next step to remove the gold plated metal.
7. The choice is yours! You can do it with Steve's AP or AR method or dilute H2NO3 method.

Good luck!

Regards
Poh


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## Juan Manuel Arcos Frank

Poh:

Nice work!!!!!!....Can you tell us about gold content in those films cartridges?

Have a nice day.

Manuel


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## pohyh

Hi Manuel

Oh ya, you shold be able to get around 10 to 12 gram of gold for each kilogram of injet printer head contact. That would equate to 1.0 to 1.2 % of gold.

The variation depend on the model of HP injet printer.

Again good luck!

Regards
Poh


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## Juan Manuel Arcos Frank

Poh:

Thanks a lot...I do appreciate all the information that you have provided to this Forum.

Have a nice day.

Manuel


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## Juan Manuel Arcos Frank

Poh:

Look,I have some information to you but I can send it to you in a PM message because it is 30 Mb..May I have your e mail?...My e mail is [email protected]

Regards

Manuel


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## pohyh

Hi All

I am back!

Just to update some of the things I have learn from this Forum. I have lay my hand on some base metal etching technique suggested by the very experience panel member namely acid peroxide (AP), poor man aqualigia (AR) as well very cools way to made gold chloride by chlorox methods.

In addition, I have also tried Nitric Acid + H2O2 (NP) as well as Nitric Acid + Sulfamic acid + Urea (NSU) as suggested by Manuel.

All the methods of base method etching work pretty well. The choice obviously depends on individual preference. Unfortunately, some form of acid fume has been generated especially when the nitric acid is been used. It simply stink!

I want to extract gold but I want to do it in a more environment friendly manner! After going through the above process, I am more determine to come out with halide etching method and I have decided to set myself a target to come out with a cook book with Potassium iodide Iodine etchant method soon!

Anyway, I have an interesting question to post for the member.

While extracting gold finger with Nitric acid with H2O2 (NP), after all the base metal have been dissolved, the blue colour liquid have decant and the gold flake have been collected using filtration method. Some of the very fine particles cannot be remove through filtration and they form a light brown mud at the bottom.

Upon adding NaoH, this mud generated ammonia gas and the process is exothermic. The mud turns to tick dark colour. May I know what this mud is?

Attached 2 picture before adding and after adding NaoH for your information.

Regards
Poh
 

Before adding NaOH




[/url][/img]

After adding NaOH



[/url][/img]


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## qst42know

Did you test these solutions for PM's with stannous chloride (SnCl) before you added the lye?


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## pohyh

Hi gst42know

Thankd for your suggestion.

The top part of the solution before lye is added should be copper, I assume since it is blue in colour. The mud probably consists of very finely devided gold which sip through the filter paper. Since it is solid particle (or more toward colloidal instead) in nature, will SnCl work?

I add NaOH to it so that I can neutralsed yje solution before I etch it again with HCL.

Anyway, I will tried it next time.

Regards
Poh


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## qst42know

I wouldn't harm anything to test while the solution was still acidic. To detect other metals of interest, palladium, or silver. It could also make certain nothing had contaminated your solution and dissolved some gold.


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## usernameguy

Hi All,
GSP, I finally got around to precipitating the gold plating solution I asked about bd10 I think the name was. It's in this thread a previous post. Anyway, you're brilliant. you're memory served you very well. I added just a bit of sulfuric, and dropped out pure gold sponge. It was a beautiful thing. Very easy to folter also since it's almost like putty. very cool Thanks a lot man. I just came across some gold plating solution that has hardly been used at all. It's "old" so the professor who comes back here like once a year wants to buy fresh every year. It again is just going to be thrown out. This solution is cyanide based, so its not the same as the last one. I'll search through the forum to see if I can find anything about this, but if your memory serves you as well as this time, let me know if there's something that will work as good as the sulfuric did on the cyanide free stuff. I know I must be even more careful with this solution as it is the cyanide that kills people. We have a well ventilated fume hood I have access to that goes through a chemical scrubber. 

Thanks again,
Guy


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## DNIndustry

Just thought Id mention this...
The danger of cyanide (outside of ingestion) is when the solution becomes acidic. The CN- Ion bonds with the disassociated H+ from the acid, forming HCN gas. Now if cyanide is ingested their is an "antedote" but A.) good luck getting it fast enough B.) dont see how a liquid in your stomach could stop a gas diffusing into your lungs.
(Thiosulfate is the antedote..supposedly)

If you are playing with H2S04 you should know that H2S gas is just deadly with no antedote.


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## usernameguy

Yeah, 
Thanks DNI. One good thing about H2S is it's very low odor detection concentration also though. I do head your warning. I actually have access to very good fume hoods that are qualified by OSAH, and are exhaused through rain scrubbers before being diluted something like 10,000 to 1 before release. Does anyone know about HCN gas detection threshhold? Is it one of thsoe super nasty's? ie., if you smell it your dead? We haves some gases here in the mustard family that are like that. arsine and phosphine. Yikes. HCN is almond smell, yes?


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## EVO-AU

Juan Manuel: I have just gone thru all the posts on this thread and quite impressed with the high exponent of knowledge with which you gentlemen indulge. I have been experimenting with 7 % Iodine on natural ores for about two years now. Very limited experience I grant you. Leaching is quite new to me in this regard.

However, my question to you is do you work with natural ores at all ? And if so, do you have anything to offer in this regard. I don't care for electronic scrap. There are just too many steps involved and I like natural things anyway. Sincerely, Phill


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## usernameguy

EVO,
I very much enjoy prospecting (placer), and have used the iodine based etchant I have access to to disolve some of my flour gold, which obviously works well. I don't have any experience with hard rock ores, but if it helps, I do know the Iodine etchant I use will dissolve up to 100g of Au per gallon. Have you had the ores assayed? I'm curious if you have free gold or sulfide complexes, etc. I do have a B.S. in geology, but not much experience. Got into the electronics/semiconductor field professionally (go figure)
-Guy


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## Juan Manuel Arcos Frank

EVO-AU:

This process was originally done in ores.It works lovely with ores but could be more expensive than cyanide process.The problem is making potassium iodide.

Regards.

Manuel


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## DNIndustry

Thats where NH4I comes in. With out looking is their anything it could complex in said ores that could create an issue?
I hate to beat a dead horse but the NH4OH method destroys KI from a $ as well as simplicity, just make more.
Juan, any insite? 
It works wonders for electronics but what about ore.
It does not attack base metals which could actually be a negative, depening on the fineness of your dirt


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## donnybrook

I live within an old goldfield. More than 100 years ago the miners were only interested in the free yellow metal. They had little time and had to make a living. Things such as mecury on copper plates were used with a stamper battery and they usually hung a bag of cyanide at the water inlet to prevent flouring of gold if they were working with hardrock.

I have a Recovery Table. I concentrate and furnace but took an interest in leaching the metals as I realized (after assaying my tailings and middlings) that even the recovery table was losing precious metals .

I have experimented with 10% iodine in 5 parts water. I add a small amount of muriatic acid (or brick cleaning acid)to keep the pH at 4. This also keeps the ORP at good levels (between 400 and 900). I have had some success with this. 

After about 24 hours using a plastic rotating drum with a length of pvc pipe weighted with concrete and sealed at either end with a cap and epoxy glue as a grinder. I process about 10 kilos or 22 pounds each time. The solution should turn a red brown.

I have been adding chrlorine or homemade liquid using dry powder for swimming pools to convert the gold from gold iodide to gold chloride. I then adjust the pH to 7 using sodium hydroxide and the metals precipitate as a black powder. Filter after 24 hours using a large nylon cooking strainer (say 8") and tissue papers over a 5 gallon bucket. Dry in an oven for about 5 hours. Roast to convert the metals from oxides to gold and then furnace or smelt.

I have never worked with circuit boards or computer scrap using this leaching method. There is supposed to be a way to recover your iodine which costs me about $40-00 (AU) to buy. I have kept the clear iodine solutions as I intend to reclaim my iodine when I know how. I think this is probably just a pH adjustment and taking the iodine back up to use again.

Base metals such as tin etc in scrap boards can cause all sorts of problems and it is best to try and eliminate these with something like brick cleaning acid before beginning the process.

Donnybrook


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## donnybrook

I am new to the web site "Gold Refining Forum". Not sure how to use it properly and have made two attempts to contact other members without success the story of my life.

A couple of references have been made to using Iodine (9%) solution to extract PM's from ores. There is a web site I am also familiar with and a link is shown within the Forum Site. I have experminted with other possible sources such as computer scrap etc in the past. Decided to use iodine as opposed to the old CLS system or another using salt and an acid. Probably for safety and health reasons.

Can someone tell me how to recover the iodine after conversion to gold chloride and precipitation. How do you recover it and then bring it back up for reuse? It seems to be the way to go from an economic point of view.

A member named Phill also had a similar inquiry.

I also table, furnace and refine.

donnybrook


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## AKDan

Donnybrook,
I am thinking based on your description that you can "recharge" and then re-use your existing solutions with the addition of Hydrogen Peroxide. If you go through the process of recovering your iodine out of solution, then you will likely need to mix back the elemental iodine into a solution of potassium iodide that you prepair to start a new leach. I believe that eventually you will need to do this anyway as every time you use the leach your volume increases and eventually becomes unmanageable.

I may be corrected on a couple of points here as I am talking from memory.


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## Palladium

http://www.freepatentsonline.com/5026420.html

The excess iodide formed during the process is reoxidized to iodine electrochemically in a special diaphragm cell to regenerate the lixiviant. :arrow: http://www.freepatentsonline.com/4557759.html



The solubility of elemental iodine in water can be vastly increased by the addition of potassium iodide. The molecular iodine reacts reversibly with the negative ion, creating the triiodide anion. :arrow: Au3+ and I- ions = AuI3, gold(III) triiodide


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## Palladium

Have you thought about bromide. Now that's interesting. :mrgreen: :mrgreen: :mrgreen:


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## solar_plasma

> That one little oxygen molecule is what prevents making the bad stuff.



What is the "bad stuff"? I do not dare to experiment with NH4I until I completely understand the dangers. NH4OH is something I normally never would bring together with iodine or silver unless I really know, what I am doing. So, would anyone like to comment this further or give a hint, what to look for?


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## kjt124

I could be mistaken, but "the bad stuff" is likely NI3 (nitrogen triiodide) which is the product of elemental iodine and aqueous ammonia. When I was younger and dumber I used to play with this stuff a bit. When it dries it makes a very touchy contact explosive. Type nitrogen triiodide into youtube for any number of demonstrations. It is rather powerful and VERY dangerous. If you believe at any point you've accidentally made some, please keep it wet (reduces the chance of deflagration). I am not certain what would deactivate it entirely. Perhaps someone else can chime in on that.

Kevin


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## solar_plasma

Yes, I know it as an experiment in ancient schoolbooks. One of the things I never felt the need to make, - even when I was a kid. I guess, my modest mind and my blood pressure has enough to do with the better documented methods. :lol: 

Thanks for the answer!


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