1st Attempt at Acid Peroxide Need bit of help

[xxmalakitexx]

Hello, I need a bit of help with the last part of the acid peroxide part if anyone can help. Everything went fine until the the last portion. I washed my gold flakes with hcl to clear off any other gunk metals, once I had them cleaned off I rinsed them and then added 1/4 cup HCL & 1/8 cup Clorox. The solution turned a very pretty yellow just like in the videos, I went ahead and filtered out the rest of the gunk, only keeping the golden liquid. After all that was done, I added very tiny amounts of SMG using a 1/4 teaspoon measure, while stirring, until the yellow in the liquid turned clear. Once it turned clear though the drop didnt really happen right away. Instead the liquid sat there clear for about 5 minutes before it very slowly started turning into what looks like just dirt water. I have waited a few hours but there appears to be very little settling if any. I removed a very tiny amount with a suction cup, the liquid appeared to be like koolaid, taking on the color of whatever it is that's floating in there. I have tried looking through Hoke's book for info but can't seem to find it. Hoping someone on here can help me figure out what went wrong and if there is a chance to fix/save it?

 

[FrugalRefiner]

You didn't mention how much gold you thought you put into solution. You have quite a bit of solution, so it may have been pretty dilute.

You didn't mention if you eliminated all the chlorine, chilled, or diluted your solution before filtering and adding SMB.

You may just need to give it some time to settle.

Dave

 

[cejohnsonsr]

Turning dirty like that is what's supposed to happen. I don't know how much "mash" you dissolved, so, like Dave said, I don't know how much gold you were expecting. Allow the solution to sit for a whole day. Then test the solution with stannous chloride. You can make your own. 1 gram tin powder (you can get it from lazersteve for $1/gram) in 30 ml HCl. If the test is positive, 1st heat the solution & allow any excess chlorine to evaporate. This can take a little while. Don't boil it & keep it covered with a watch glass. If there is enough SMB still in the solution you will see it turn dirty again as the chlorine is driven off. If you get down to about 1/2 the volume of your solution & it still hasn't turned dirty, let it cool completely & add more SMB. I mix mine in water before I add it to the AuCl. The General Reactions List says 65 grams of SMB will saturate 100 ml of water. SMB is cheap & it won't hurt if you use a bit too much. When you're all done, make sure you let it settle for a whole day. It takes a long time for the tiny (microscopic) particles of gold to settle to the bottom. After a couple of hours you'll be able to see it better as the top of the solution begins to clear That brown powder in the bottom is your gold. Patience, my friend. You'll see. It's pretty cool to watch.

Ed

 

[xxmalakitexx]

Thank you for the reply guys, also my apologies for not putting the correct amount of liquid/gold used before-hand. I only had a small amount of gold...roughly 2 grams. I believe Dave may be right and I added too much water to my solution. I had 2 cups of liquid gold then I added 2 cups of water to dilute. Too much water now that I think about it...I just stepped outside to check on the solution. It is finally starting to settle so the murkiness is going away, powder/gold? is starting to form at the bottom. I hope you dont mind me asking, but I saw on another post that Mason jars were bad idea to mix/process in? Is this true? Again....thank you so much guys....

Gio

 

[cejohnsonsr]

Yeah, Mason jars heat up ok once or twice, but they don't hold up well to the thermal shock of cooling down too quickly. You really need a couple of borosilicate beakers. And for a watch glass I found a flat glass candle stand at WalMart for $2. It covers a 1000 ml beaker just right & is cheap.

I just looked at your pic again. Yeah you want to evaporate quite a bit of that off. You'll see when it happens. I made the same mistake with my 1st batch. Had so much solution that I had to split it between 2 beakers. 1 dropped & the other didn't. I was REALLY confused. Chlorine was the problem. I even reheated the beaker that had dropped as expected & got a little more. Be patient all the way through. Let it evaporate about half, but don't let it boil. Then let it sit & settle for a whole day. 24 hours. Go away & find anything else to do. (I swear that part fascinates me but it happens so slow that it almost kills me. LOL!)

Ed

 

[xxmalakitexx]

Ah ok, I will stop using these immediately and order some beakers.I will have to keep myself entertained for the next 24 hours hahaha.Thanks for the tip, I will hit walmart for that component. I understand what you mean, I have spent most of today just staring at the chemical reactions. Its been fun even though I fudged up a little bit but I suppose it could have been worse.

 

[Anonymous]

Ah ok, I will stop using these immediately and order some beakers.I will have to keep myself entertained for the next 24 hours hahaha.Thanks for the tip, I will hit walmart for that component. I understand what you mean, I have spent most of today just staring at the chemical reactions. Its been fun even though I fudged up a little bit but I suppose it could have been worse.

At this point a watch glass is something you might have at home. If you have a saucer or small tea plate, that's what you need right now. The thing you need to get are different size beakers (heat resistant). I don't have a watch glass at all, but I use some old tea cup saucers that we never used before that were given to my wife and I.

And to confirm, for the amount of gold that you were expecting to recover, you put in wayyyy too much water.

That mason jar,... if it makes it through tonight or however long it takes you to precipitate the gold, don't use it no more for heating anything you're refining. I did it once myself (not a mason jar though) and the bottom of my jar cracked and broke around the bottom of the complete jar. When I lifted the jar up, there was no bottom to it. It was laying inside the catch pot I had setup, just in case.

On another note: I've bought 3 of those warmers from the Goodwill last few months ago. They're good if you have the heat rated glassware, but I see that you don't have a catch pot/container under neath it in case it happens to break, like mine did. I didn't lose anything. I bet if your glass breaks, you're going to lose everything. Get a catch pot/container... just in case.

Also, from what I tested so far on those warmers, they will get to a temp of approximately 180F. That was after 35 minutes of mine being on. It won't get to a boiling point that I know of, but they're a really good thing to have to heat small glass solutions without using a hotplate. The only downfall with them is that they have no temperature control. It's either off or on. So, be careful when using them, and get as many as you can afford. They're worth it.


Kevin

 

[Geo]

guys, i for one am fond of Mason brand jars. i feel it is perfectly safe to heat and even bring liquids to a boil (i dont recommend boiling in a mason jar,im just saying that i have before) in a mason jar as long as the jar is in a pyroceram casserole dish. always remember the catch pan. sturdy plastic for cool solutions and pyroceram for hot solutions.

 

[butcher]

My most of my lab-ware is canning jars, 2nd hand coffee pots, plastic buckets...
Normally I do the heating in the ceramic casserole dish, or coffee pots, and not my jars, I will use the jars on electric hot plate coffee mug warmers directly quite often and never had a problem, and will boil in them but only with a water bath, sometimes that water bath can be a solution I wish to evaporate down (like a waste of saltwater solution...).

I use a gallon pickle jar that sits in a sand bath for a distilling rig, personally I never put the jars on a very hot surface directly, (I use liquid or sand to distribute heat evenly, raising and lowering heat gradually).

The canning jars can take a lot of heat, but the heat needs raised slowly and lowered slowly, raising or lowering the heat too quickly thermally shocks the glass, and the heat has to be fairly evenly distributed hot spots can cause it to crack, a jar sitting on a very hot surface and cool sides of the jar the jar will crack right around the bottom, this can be worse if solids are in the bottom of the jar filled with liquid, if you hear a jar of any lab glass crack, do not lift the glass, leave it there, use you suction tool to remove liquid to another vessel before trying to lift the cracked glass.

Geo I do not doubt one bit you have boiled liquids in these jars sitting in a casserole dish directly, I just wouldn't try it myself, But I will boil in them using a liquid or sand bath, being very careful not to thermally shock the glass.

 

[Geo]

thank you Butcher.yes, of coarse use water or sand.i always do and forgot to mention it. for some reason, the price of gold had me scatter brained for awhile. you can slowly raise water to a boil in a jar. if you want to try something really cool, get one of those 5 penny paper bags that doesnt have a hole.fill it with water and place it over a burner or even in a small fire and watch the water boil without burning the paper bag. i know this means nothing to the conversation but it is kind of cool to play with. :lol:

 

[xxmalakitexx]

So I went ahead and waited a lil bit of extra time extra 12 hours to make sure everything dropped from my solution. I messed up on the first part like I stated before, added too much water but thanks to crazy Texas weather it has evaporated a good chunk. I will try and get a picture up a little later, once i filter the gold, waiting on weather to brighten up, went from 92 to 75 in a couple of hours and rain is heading in. Made sure to properly cover everything to avoid any nasty rain water getting into my solutions.

Thank you for all the back info on the mason jars as well, after the last message I went and checked on all the info for the mason jars I am/was using. They are heavy duty canning jars, glass is close to a 1/4 in thick & tempered, they were designed to go into a pressure cooker which gets hella crazy hot. None the less I will start using some sort of safety catch, just in case something does happen and the bottom happens to crack, just because its improbable doesnt mean its impossible from happening. I have avoided bringing ANYTHING to a boil, at the most it would maybe get close to boil, though I will still take the advice and obtain some sand to use as a buffer between the jars.

Def agree with you Kevin, a lot of the stuff that I am using now, I have picked up some Goodwill. The little heaters I run across all the time for about 2 bucks, as well as old coffee pots for about a dollar. I have even seen some of the mason jars there,the ones I have now I obtained from my mother-in-law. Lots of good things for reasonable prices for anyone who is looking.

 

[xxmalakitexx]

So finally managed to evaporate the left overs and this is what I was left with. I am sure it is not the best purity, looks still rather dirty even after hcl bath, but i am happy, I mean it doesn't look too bad.....does it? I learned a lot more about the process and hope to refine it down later on. For now i am going to stick to very small batches until I get it down right.

 

[TomVader]

If you are planning to make your own Sncl, I have used 95/5 tin solder and lead free fishing sinkers (tin) both with great success. With the solder you end up with undissolved antimony in the bottom of the container but you can just decant into another container. Does anybody know of a practical use for antimony?