First batch EVER..................DISASTER!!!!

[carasoph]

Hiya all,

Well, I've been strolling here for months now, gathering data, making notes to myself, exploring and I even made a booklet for my days as a refiner, where I wrote a step-by-step ways to remove EVERY source in the best way. I even wrote MUST DO and NEVER DO checklist so that I wouldn't end up losing chems, time, materials and even my health...

This morning I woke up saying to myself - "Today I'm gonna give it a go and have my first batch....a small one just to see if I got it all right..."
You see - my wife and son are on vacation visiting her family..... PERFECT opportunity!!!

I took several fingers I had stored for 2 years now (about a dozen) and put them in a lab pitcher, 1 liter of size.
I put the pitcher in a plastic container for JUST in case...I never thought I'd need it...
The minute I opened the NEW, LAB grade, 1 liter bottle of 32% HCl, I had a bad feeling about this... there were fumes coming out of that bottle the second I opened it.
I said to myself - "well it's a lab grade, so it's OK...
I covered the fingers with the HCl (about 250ml) and there was a slight reaction - just a few fizzes and a whole lot of fumes.... :shock:
I've opened the 30% H2O2 bottle to put inside 1/3 of the HCl and poured... I only got to pour about 30-40ml and the whole thing went overboard - right into the plastic container (THANK GOD I had the sense of putting everything inside................
Well, needless to say that I had to flee from the house along with my dog, but not before I poured the whole thing into the container itself and diluted it with 3-4 liters of water...
I came back home an hour later, and the air in the house had a little chlorine in it - but not more then the Household Clorox as if I cleaned the house...
When I went to check on the batch - I found that there are MANY flakes floating, and only a few fingers still had gold on them.
I started filtering it - and it took me almost 90 minutes to filter it....

So -
30 seconds of stripping - V
90 minutes of filtering - V
Experience - SCARY...
Lesson learned - DO NOT USE A 30% H2O2 with 32% HCl, and NEVER.......NEVER do it at home !!!


Does any1 has a good way of filtering this (I use the same method Steve show in the videos - but it takes too long - about 2 liters per hour)...

Caramon

 

[jsargent]

Just a bump in the road amigo. Sounds like you just need a couple of items to solve the problems. FIRST is ventilation. Do it outdoors or install a fume hood. Always wear a good respirator. The type with cartridges specific for acid fumes. Second is slow and careful titration. H2O2 is powerful stuff and a little goes a long way.
Never give up! :wink:

 

[qst42know]

In my experience it's normal for HCL to fume when exposed to air.

However First aid peroxide of approximately 5% is effective for making AP. I would suggest diluting your peroxide before adding it.

I would also urge you not to do this indoors without an effective fume hood.

 

[carasoph]

Hiya all,

I figured that the H2O2 concentration was WAYYYYYYY too strong from its reaction... :lol:
This time I diluted it to around 11% (it was 1 liter 33% - 2 parts water + 1 part H2O2).
Another different thing I didn't do was -----> NOT indoors... I went to a remote place (I don't have a yard... ) and performed the test.

similar quantities, but the 11% H2O2...

It started good - fizzed a lot and produced a yellow-green foam on top.
a few minutes later (15-20) it stopped foaming and only bubbles remaining,
when they got weak - I added a little H2O2 to rejuvenate the AP... fizzed some more and again..the whole process again - I ended up adding H2O2 3-4 times till I saw no more gold on the fingers.
The whole thing took about 90-100 minutes.

The thing is - I used the same amount of fingers and I ended up with A LOT less flakes - I think I dissolved some gold into the solution.

1. Unlike the first try - THIS solution turned out Emerald green, the first turned Sky blue - any ideas why ?!? (I know that copper creates this color)
2. Would H2SO4 (98%) be OK for the AP procedure ? (instead of HCl I mean...)
3. I filtered the solution using a Viscose fabric cause I couldn't find any decent paper filter - mine are disintegrating after 2-3 times I pour solution on them... :x

I think that next time I'll use a 20-22% H2O2 when I'm outside again - it takes a LOT less to finish...

Thanks,

Caramon

 

[Platdigger]

I am most certain you disolved gold.

This only needs 3 to 5 percent peroxide just to get the proccess going.
After enough copper gets disolved into solution, it is then the copper chloride that does the etching.
It is to work slowly.......
You should check out Lazersteves site.
Randy

 

[qst42know]

You will need to test your solutions for gold. AP solutions heavy on peroxide (even 5% peroxide) will dissolve gold.

 

[goldsilverpro]

I agree. Use Steve's proven method using the 3% H2O2. It takes awhile, but it works. He's covered it in detail many many times on the forum.

 

[carasoph]

Thanks for answering...
I do not have the testing solution yet - I need to get my hands on tin... I understood that the soldering tin wouldn't be good for the job...
I saved the solutions in separate containers (closed brown glass bottles) till I do have the solution...

But what about the acid? would an H2SO4 98% be a good replacement for the HCl? (My guess is - NO..... no Copper Chloride will be formed, but I'm just checking... )

Thanks a million..

Caramon

 

[EDI Refining]

FYI -You shouldnt be doing this in your house, without a fume hood

 

[qst42know]

If you are in an apartment you might want to check on a window box. Perhaps that may work for you.

 

[Juan Manuel Arcos Frank]

Shalom Aleichem,Carasoph:

I am glad that you have done your first gold recovering,Congratulations!!!!!!.

Do you still have that H2O2 (30%)?Do not be scared.I just want you to make a little experiment to save the World.

The sky blue solution you got is a cooper salt (probably copper hydroxide) because copper promotes H2O2 decomposition.Copper hydroxide is insoluble in water but soluble in acids (like AR).

Would you do the experiment for me?.The experiment is easy,safe and will help all Forum`s Members.

Have a nice day.

Manuel

 

[qst42know]

I just checked the peroxide I have been using and it is 3%. It works just fine but I can leave it sit for as long as it takes.