Issues with 1st AP attempt --- Need your help

[ahmadbayoumi]

Hello ALL,

I went through my 1st real attempt for processing about 52 RAM fingers.

ALL step were exactly as it should be with the expected end results except the gold precipitating step.

1st I trimmed the RAM fingers.
Then added HCL + copper chloride II (come from previous trail attempt)
Then left the whole solution for about 2 days with air bubbler.
Then after ALL gold foils went into the dark green solution, I filtered the solution leaving the gold foils behind in the reaction container.
Then washed the gold foils using HCL (2 washes) then water.
Then added HCL(200 ml) +CL (50 ml) till all gold foils dissolved and a clear and yellow Auric Chloride has been formed.
Then tried to precipitate gold with SMB solution (100 ml water + 65 gram SMB).
At this step, the 1st thing happened was just a dirty brown solution started to form then nothing else.
then I added more SMD then more and more till I finished the whole 100 ml of SMB solution but still nothing but small and muddy brown particles.
then I added more SMD powder but sill nothing occurred but the solution was fizzing.
then added more SMD but only fizzing.
Then I left the whole solution for the whole night and at the morning I noticed that the solution went yellow again but not as shinny and clear as before.
Here, I though I added more than it was need from the CL and though that it may help heating the whole dirty yellow solution to liberate CL.
I was expecting to see white chlorine gas smoke but it was not the case and the solution still very light and dirty yellow

I don't know what went wrong here and how to fix this and I need your help here please.

Is all of this was due to excess CL and if so how i can over come this ?

 

[FrugalRefiner]

Hello ALL,

I went through my 1st real attempt for processing about 52 RAM fingers.

ALL step were exactly as it should be with the expected end results except the gold precipitating step.

1st I trimmed the RAM fingers.
Then added HCL + copper chloride II (come from previous trail attempt)
Then left the whole solution for about 2 days with air bubbler.
Then after ALL gold foils went into the dark green solution, I filtered the solution leaving the gold foils behind in the reaction container.
Then washed the gold foils using HCL (2 washes) then water.
Then added HCL(200 ml) +CL (50 ml) till all gold foils dissolved and a clear and yellow Auric Chloride has been formed.
Then tried to precipitate gold with SMB solution (100 ml water + 65 gram SMB).
At this step, the 1st thing happened was just a dirty brown solution started to form then nothing else.
then I added more SMD then more and more till I finished the whole 100 ml of SMB solution but still nothing but small and muddy brown particles.

It sounds like everything went as it should have. When your solution turned dirty brown, that was your gold being reduced to metallic gold. The small and muddy brown particles are your gold. You added way too much SMB. As a general rule, you only need one gram of SMB for each gram of gold in solution. You would not have 65 grams of gold from 52 RAM fingers.

then I added more SMD powder but sill nothing occurred but the solution was fizzing.
then added more SMD but only fizzing.

That's what SMB does when it's added to HCl. It fizzes. The acid causes the SMB to release sulfur dioxide gas, which is what reduces the gold to metallic form.

Two things stand out to me in your procedure.

First, you didn't mention heating your pregnant solution or allowing it to sit for 24 hours before adding the SMB. This allows any excess chlorine to escape from the solution before precipitating your gold.

Second, you don't mention testing your solution with stannous chloride anywhere along the line. Without testing, you'll never know whether you have gold in your solution or whether it has been completely precipitated.

If there is still some brown powder at the bottom of your solution, that's your gold.

Dave

 

[ahmadbayoumi]

Thanks Dave for your reply

I did heated my solution but after adding the SMB not before adding it .. Does it make any difference for heating before of after adding the SMB ?

Yes .. seems I added more SMB than it was needed but this was because I have seen some posts here saying that adding more SMB would overcome the excess chlorine.

How this much SMB may affect the process ?

However, I didn't make my test with stannous chloride but there must be more gold that hasn't been precipitated yet because there were much more gold foils.

So the question now for me .. Where's my gold and how can I reclaim it from the current solution ?

 

[MarcoP]

Looks like you didn't removed nitric excesses.

 

[ahmadbayoumi]

Thanks MarcoP for your reply but I didn't use nitric acid

I was using AP process not AR .. 8)

 

[bswartzwelder]

Why did you use copper chloride II from a previous trial? I am making the assumption that trial was a failure for one reason or another. You may have contaminated that trial and by reusing it to start this batch, you may have carried those contaminants over into this batch. HCl and peroxide are 2 of the cheapest chemicals you can get for recovery and refining.

For 52 RAM fingers, 200 ml HCl is WAY TOO MUCH.

Next, you should have heated to solution to drive off the excess chlorine or left it sit to drive off the excess chlorine. A stannous test at this point will tell you if you have any gold in your solution. You would expect a positive result.

Then, to precipitate, you used 100 ml water and 65 grams of SMB. That was enough SMB for 2 ounces of gold. The dirty brown solution (and the brown mud) which fell to the bottom of your container was your gold. Gold recovered in this manner is a brown powder and not a miniature ingot or pellet. You should have left it settle and then decanted as much of the liquid as possible at this point.

After adding the proper amount of SMB, the solution should have lost its golden yellow color. Another test with SMB at this point should have been negative. A negative test indicates all your gold is in the mud.

If your solution has turned yellow once again, why haven't you tested it to see if it contains gold?

It is painfully obvious that you haven't been reading the Forum and Hoke. If you would have, you would have known the answers to everything here. Recovering gold from finger foils has been covered in quite a bit of detail hundreds of times. It is one of the easiest and most fool proof things you can attempt.

You really need to set everything aside and start reading Hoke and the Forum. Without testing, you may still have gold in solution. You simply cannot tell without a valid test.

 

[FrugalRefiner]

I did heated my solution but after adding the SMB not before adding it .. Does it make any difference for heating before of after adding the SMB ?

When you dissolve your gold using HCl and clorox, the clorox releases chlorine which oxidizes the gold which then combines with the HCl to put your gold into solution. There's usually some excess chlorine left. If you try to precipitate your gold, it will redissolve. Heating the solution will drive off the excess. Leaving it sit for 24 hours will also work.

Yes .. seems I added more SMB than it was needed but this was because I have seen some posts here saying that adding more SMB would overcome the excess chlorine.

It's better to get did of the excess before adding the SMB.

How this much SMB may affect the process ?

Adding too much SMB will contaminate your gold solution and lead to contamination of your precipitated gold.

However, I didn't make my test with stannous chloride but there must be more gold that hasn't been precipitated yet because there were much more gold foils.

If you don't test, you're just guessing there is still gold in solution. Testing will tell you if your guess is right or not.

So the question now for me .. Where's my gold and how can I reclaim it from the current solution ?

My guess is, it's on the bottom of your container. Foils from fingers look like a lot of gold, but the foils are only about 30 microinches thick. 30 microinches. A microinch is one millionth of an inch (.000001 inches). 30 microinches = .00003 inch thick. A human hair is about 3 thousandths of an inch (.003 inch). So if you had the instrument needed to measure it, you'd find that a hair is about 100 times the thickness of those foils.

Make some stannous and test your solution to see if there is still gold in solution. Don't be fooled by a "false positive". That's another consequence of using too much SMB.

Dave

 

[ahmadbayoumi]

Thanks a lot bswartzwelder for your reply

Why do you assume that I didn't do my home work and didn't read ?

I really Spent 100 of hours reading and searching the forum and even watching 10s of vids about gold refining.
Yes .. I didn't read the whole Hoke but have read many sections and compensated the rest by other readings.

Asking questions doesn't mean I didn't read and study .. but always there will missing parts that need more and more reading and consulting experts.

And that's what I'm doing here in this great forum

I know some people do the refining without any knowledge about anything and they are successful and I can simply pay some money and they can teach me what they doing.

But I don't like such easy ways .. I prefer to learn and do it with knowledge even if it tack months.

I didn't make stannous chloride tests because I'm unable to find it now but I'm sure about its importance.

I didn't use H2O2 with HCL and instead used copper chloride because CuCl2 is the active ingredint in the ecthing process and H2O2 is just an oxdizer and this was the new method developed by samuel-a and posted here in the forum.

I know that there must be another gold that hasn't be precipitated yet because the gold foils were quite good amount.

I'm attaching here some pics for my experiment

 

[ahmadbayoumi]

Thanks a lot FrugalRefiner

Seems that testing with stannous chloride is a must here so I'll try to find other stores that may have it.

But as I added to much SMB, how I can avoid false positive test ?

Also, now I knew that heating should have been done before trying to precipitate gold but does it worth now if I tried to heat the solution after the addition of SMB ?

 

[Claudie]

Looking at the solution as it is sitting after the SMB was added, I think you just need to let it settle. The amount of Gold from 50+ finger boards isn't going to be a great deal. The foils you had, after washing, most likely still contained Nickel.

See this post: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=21063

EDIT:Spelling

 

[maynman1751]

Do a search here on the forum for making stannous chloride. It's simple. You need to get some 95/5 solder (95% tin/ 5% antimony) and dissolve some in HCl.

 

[g_axelsson]

You can make tin chloride with 60/40 tin/lead solder too, most of the lead chloride will just drop to the bottom as it's not that soluble. If you are concerned with the lead, just chill and filter and by all practical means it is as pure as it needs to be.
Just as a test I made some tin chloride by dissolving the solder from a circuit board with components still on... it worked.

Collect the solder from the memory sticks you have, mix it with a little bit of HCl and wait until it dissolves. Now you have your testing solution.
You should also take the fingers from one ram stick, run it in your copper chloride until the foils are loose. Use these foils to make gold chloride. Save this as your gold standard, test your tin chloride against it every day to see that the stannous chloride hasn't gone bad. (oxidized)

Tin chloride is one of the easiest chemicals to make in refining, there are no excuses for not testing a problematic solution. Whenever in doubt, test!

... this is at least the fifth time I write down this procedure and I'm far from alone. It's been written down countless times already. Use the search button and read some more.

Göran

 

[FrugalRefiner]

Seems that testing with stannous chloride is a must here so I'll try to find other stores that may have it.

As others have said, there are many ways to make stannous. Use it every step of the way and you'll always know where your gold is.

But as I added to much SMB, how I can avoid false positive test ?

Once you've added too much SMB, you can't really avoid a false positive, you just need to be aware of it and how to recognize it. A search should turn up plenty of good results.

Also, now I knew that heating should have been done before trying to precipitate gold but does it worth now if I tried to heat the solution after the addition of SMB ?

Heating before you precipitate helps to drive off excess chlorine that can interfere with the precipitation. Heating after the gold has been reduced can help it to agglomerate and drop cleanly. Keep studying and it will all start to come together.

Dave

 

[goldsilverpro]

In the photos, "Muddy dirty brown solution after adding SMB", all of the brown color is gold. just let it settle and collect it. That exact, particular blue color of the solution in those same photos indicates to me that all the gold has dropped. Definitely test with stannous chloride but I don't think it will show anything. I think all the gold has dropped. You didn't start with much and you won't end up with much.

 

[Pantherlikher]

I see 2 of the biggest "newbie" mistakes as usual.
First, you need to test prior to SMB. Doing this important test will tell you right away if there is any excess CL. Which if present, will redissolve gold.

Second and more important... Total lack of patience present.

Even without heat, CL will dissipate from the solution with time and patience.

Guess at how much SMB it will take to drop the gold. Usually way over guessed weight but ok.
Do Not add more just because you did not see a brilliant dance of magic before your eyes. PATIENCE

Instead of running back to the forum and asking what's wrong, Come here and do a search of gold drop. Narrow the search with questions about drop but it would be allot better for you to read every post.

This exact "Need your help" AP, gold drop problem has been addressed too many times to count.

I had this very problem and so did a search, found my answers and learned far more then just my "problem". I then decided to wait...2 weeks untill I saw brown mud finally show on the bottom of my solution. Which brown mud is what gold looks like when drops the first refine/drop after collecting/concentrating.

B.S.
READ!!!

 

[bswartzwelder]

When you make stannous chloride test solution, it will go bad after a period of time. This is normal. It happens. Most people make a new batch of stannous about once a month. As an alternative to re-making your stannous solution it is always a good idea to test the stannous chloride solution before using it.

I purchased a small bottle of gold chloride on the Internet. Every time I want to use my stannous chloride, I dip a Q-tip into the gold chloride and then drip one drop of my stannous chloride onto it. If the Q-tip changes to a very dark color, I know what to look for when I test my unknown solution.

I have also made a stannous chloride solution which doesn't seem to go bad. I have been using from the same bottle for well over a year now and it still seems to work as well as the day I made it. I have purchased some pure tin pellets from a seller on eBay, and stannous chloride (anhydrous) powder from another seller on eBay. I put a small amount of HCl in a small brown bottle with a stopper. Then I added a half dozen or so small crystals of the crystallized stannous chloride. I also put 1 or 2 of the tin pellets into the bottle and shook everything. I keep the small brown bottle in my refrigerator in the area where butter is supposed to be kept. My grand children cannot reach it when the come for a visit and my wife knows what it is and doesn't bother it.

If anyone uses the search function on the forum and enters "brown mud" more than 10 pages of references comes up. Reading and testing are the best ways to learn.

 

[ahmadbayoumi]

Finally and after waiting for more than 5 days I managed to precipitate some brown gold powder.

It's much less than I was expecting but I think it's good for the 1st trail.. Isn't it ?!

Yes Pantherlikher, I was not patient and that's the 1st lesson I learned from my 1st useful experiment and I can summarize below my mistakes:

1- Gold foils loss in the reaction container; Very small gold foils was attached to the container and I was unable to release these foils ... need your advise here.

2- Gold foils loss in the filtering beakers; Very small gold foils was attached to the beakers and I was unable to release these foils ... need your advise here.

3- Using 2 beakers to filter the gold foils; ONLY one big beaker should be used to minimize losses

4- Adding more Clorox than it was needed; Clorox should be added in small increments.

5- Heating after adding the SMB to free excess CL; Heating should be prior to adding the SMB

6- No Stannous Chloride tests performed; Tests should be performed at each stage.

Now, I'm still having the solution (supposed AuCl2) and still haven't done the stannous chloride test .. I'll make this test in the next few days to make sure that all gold has been already precipitated.

I'm attaching a pic for the precipitated gold powder (still haven't the change to weight it) and i need your point of view.

Now, I have a question; I can still see very thin and fine particles that haven't been settled in the bottom and I'm unable to collect them .. How should I deal with this?

The 51 RAM sticks original weight was 870g.

Will try the RAM IC chips in the nest few days to have an overview about the whole RAM yield.

Thanks a lot Claudie for the link, it was very useful.

However, still was expecting much more .. correct me if I'm wrong.

Thanks a lot maynman1751, g_axelsson and bswartzwelder for the information you provided about how to make stannous chloride
I have read many posts about the same after doing a quick forum search.

Thanks a lot FrugalRefiner for your reply .. it helped me a lot to identify some of my mistakes

Thanks a lot goldsilverpro for your useful reply but I can't see the blue color you are referring to.

By the way Pantherlikher what do you mean by "2 weeks until I saw brown mud finally show on the bottom of my solution."

Do you mean after adding the SMB you have has to wait 2 weeks for fully precipitate the gold ?

Thanks all of you for the great support I'm always having here

 

[Claudie]

What is the weight of the powder.
Don't forget to practice Harold's washes!

 

[patnor1011]

Amount pictured looks about right. It will be actually even less after second refining as it is still contaminated.
52 RAM stick are about 50-60 grams of fingers. Since you use metric, yield from fingers can be anything between 4-8 grams from kilogram. You may expect about 0.3-0.4 grams of gold from your experiment. Since you mentioned some foils stuck on equipment along the way I would say 0.2 g.

 

[ahmadbayoumi]

Have washed the precipitated gold powder with HCL (2 washes) and water (2 washes)

So not sure if Harold's washes! are different that what I have already did.

Also still didn't wight my gold powder .. will weight it and share with you