broken jar

[clint s]

help please ok I Iearn a good lesson today, like a dumb ass, I well ok i had 100 grams of scrap and 4 grams of 14kt I was processing i started with soaking the scrap in nitric with h2o
over night ,then i filterd of tha remaing metals ,made my ar solution then put the metals in and let them do there thing when it was done i pooured off the ar then put what was left in a fresh ar solution when it was done i started to boil all of the solution with it just enough heat to boil ,it was coming to a syrup i was reducing heat and the next step i was following the direction of hokes
to add hydrochloric to reduce the nitric that was in the AR and my jar cracked well you can guess what happened next ya. ar solution and fresh hydro every where on my wifes new glass top stove ,so the first thing i did was to pour baking soda on all the Ar all over the top of stove lucking it has a lip all around it, so the AR stayed on top, as i was pouring the baking soda {sodium bicarbonate on top i could see brown clumps forming on the top of SB i was guessing it was the gold not sure but this is where i am at i scraped all of it up and put in in a new container and added lot of water , i got most of the foam and clumps all in my container what can i do to save this terrible mistake and good lesson learned ?glad i had good vent a hood

 

[skeeter629]

Clint,

If you are doing this in your kitchen, are seriously doing it wrong. You are puting your life in danger and the lives of your family. You should reconsider refinging until you have the proper place to do it.

 

[jimdoc]

If you were doing this in your kitchen, you haven't read enough about safety.

Jim

 

[patnor1011]

Ok at least he said what he did. Clint you can bet that you damaged your "hood" (kitchen air digestor) with fumes from nitric and AR reacting with metals.

 

[clint s]

well i have a garage and a hood system set up for welding ,stainless vent a hood .my wifes stove just got here and i put it in garage till we could get in installed ,and i didnt have my hot plate yet so thought glass top even heat so unboxed ,wife not knowing a thing or she would of killed me proceded with my refining with my first batch and dumb move i guess .
do i put the hydro in when it is still boiling or wait till it cools ? and know how do i finish with what i have left is my gold lost or do i have a chance to get it still?

 

[Harold_V]

i started to boil all of the solution with it just enough heat to boil ,it was coming to a syrup i was reducing heat and the next step i was following the direction of hokes
to add hydrochloric to reduce the nitric that was in the AR and my jar cracked well you can guess what happened next ya. ar solution and fresh hydro every where on my wifes new glass top stove

Surely, you're joking, eh?

No one in their right mind would process gold in a kitchen, where fumes will destroy eveything of value, and do it in short order.

Edit: I just read your follow-up post, so I understand that this was not done in your kitchen. Aside from that, my comments still stand. Ducting acid fumes with stainless steel will slow corrosion, but not stop corrosion.

As for the stove---this isn't something you can hide from your wife. That pretty white cook top is now going to be purple, and your chance of getting it cleaned isn't good. Further, anywhere the gold chloride solution made contact with exposed metal, you can expect that there will have been metal sacrificed as gold was cemented. For all practical purposes, it is my opinion that you trashed the new range. I hope you can prove me wrong.

I read that you "boiled" your gold chloride solution. That isn't acceptable, not now, not tomorrow, not ever. When you evaporate, do NOT USE THE TERM BOIL! You are evaporating, not boiling.

I'm up to my eyebrows with you guys that resist learning proper terminology, then open your yaps discussing the errors of your way, passing on to others the ongoing misinformation that gets them in trouble.

glad i had good vent a hood

Had!

Yep, that's the way I'd look at this matter. You had a good hood. It no longer is. Kitchen hoods are made of metals that are readily destroyed by acid fumes, in particular, the aluminum screens that capture oils. Rarely are they ducted outside---they generally have a filter and recycle the air, to prevent heat loss. Does yours? If it is ducted to the out-of-doors, is it ducted in galvanized steel? If it is (make that was), you have new effectively destroyed the tubing.

You really need to stop doing foolish things and start reading Hoke, so you have a better understanding of what you're doing, and what the consequences are of ignoring advice that is readily available on this forum. Refining in your kitchen has never been endorsed. Now you know why.

Harold

 

[clint s]

every thing is ok it has a glass top and cleaned up perfect the solution did not come in contact with any metals at all just glass thanks for all the help every one .for my hood i weld with it all the time it wont hurt it if it doesi will put new one in

 

[clint s]

hokes book it says now boil the solution down gently as i was

 

[Harold_V]

hokes book it says now boil the solution down gently as i was

My copy of Hoke is in storage, so I can't verify what you're saying, but I can explain in fine detail what's wrong with "boiling", even gently. It is the cause of lost values, with evidence easily found if you discharge the fumes on a surface----like the side of your travel trailer.

I got baptism by fire in that regard, when I started refining and didn't understand the importance of slow evaporation. Like you, I boiled at a low heat, although I ducted the vapors with a window fan instead of a hood. What a lovely pattern I created in purple, which was removed by rubbing compound.

When evaporating, the solution should NEVER boil, and you should never make reference to boiling when you're talking about evaporation. All too many take it literally.

I'm keeping a good thought where your new range is concerned. I would expect at least some staining and damage---if you dodged that bullet, you're a fortunate man.

Harold

 

[Emmjae]

hokes book it says now boil the solution down gently as i was

I'm afraid he is correct. I just grabbed my hard copy of the book. Page 44, section (5), in the 3rd paragraph. "Now boil the solution down gently, to a syrup, being careful not to spatter." She uses the term "evaporation" throughout the rest of the process.

 

[clint s]

I wondered if you would lose metals or the gold when evaporating the solution at a boil also where does the base metals go this is a question i have .

ok first i used just nitric to get most of the base metals dissovled did that twice till the nitric would not react anymore poured off the remaining liquid with filter then took the metals and put them in the AR solution mixed 4 to 1 pour just enough to cover metal did that twice then started to evaporate at slow boil at this point where does the base metals go ?

in the solution or to bottom of beaker as the solution evaps off do they go into the air ? i think evaporating off the solution isnt a good way is there a way to percipating the gold with out evaporating the solution or is that a must with that process .

also on my new range it was all glass top or i would of had to trash it i am sure ,it cleaned up perfect , as the bottom of the jar broke i only had about a inch and 1 half of solution in jar
and it spread about 10 inches around soon as i put the baking soda on it ,it contained it ,i alwasy keep fresh SB close when i am working with acids good thing or it could of been worse, i have a big pile now of pea green sluge as it settles i have been pouring off the water as it drys the white soda shows can i put the sluge in new nitric or how should i procced when the powder is all dry ?

 

[Harold_V]

I wondered if you would lose metals or the gold when evaporating the solution at a boil also where does the base metals go this is a question i have .

It isn't selective---the loss isn't because of evaporation, but because of the effervescence that accompanies evaporation at a high temperature. The tiny bubbles that rise out of the fluid carry with them traces of the solution, likely in equal balance, so both base metals and gold are lost.

ok first i used just nitric to get most of the base metals dissovled did that twice till the nitric would not react anymore poured off the remaining liquid with filter then took the metals and put them in the AR solution mixed 4 to 1 pour just enough to cover metal did that twice then started to evaporate at slow boil at this point where does the base metals go ?

Any base metals that were not removed in the nitric dissolution are dissolved in the succeeding operation, with AR, along with the gold. The exception is silver, which is primarily converted to silver chloride. The base metals follow the gold chloride through the process, and are separated when you selectively precipitate the gold. The problem is, when you precipitate gold from a dirty solution, you can expect drag down to include traces of the base metals, which may or may not wash out well afterwards. Gold precipitated from dirty solutions often requires a second refining to raise its quality.

in the solution or to bottom of beaker as the solution evaps off do they go into the air ? i think evaporating off the solution isnt a good way is there a way to percipating the gold with out evaporating the solution or is that a must with that process .

By using the procedure you described, where you covered the values with acid, you most likely will have to evaporate---because you are using too much acid. Evaporation, unless you intend to concentrate your solution, isn't a requirement, so long as you have no free nitric acid. One evaporates to eliminate free nitric, which hinders the precipitation of gold, plus can be troublesome when attempting to wash the recovered gold.

also on my new range it was all glass top or i would of had to trash it i am sure ,it cleaned up perfect , as the bottom of the jar broke i only had about a inch and 1 half of solution in jar
and it spread about 10 inches around soon as i put the baking soda on it ,it contained it

That may well have absorbed and neutralized the gold chloride, but any traces that remain on the surface will be photosensitive and will turn purple in time. If you dodged that bullet, I believe you will be fine. Any scratches that may have been in the surface will be subject to staining, too.

i have a big pile now of pea green sluge as it settles i have been pouring off the water as it drys the white soda shows can i put the sluge in new nitric or how should i procced when the powder is all dry ?

I'm not sure what you mean by "sluge". Do you mean sludge?

It's clear you don't understand what you're doing. You really need to concentrate on the reasons you do the things you do in the process of refining. When you understand why, it's easy to know what to do.

Pouring off solutions isn't a good idea. You would have been best served in this instance to simply recover everything by placing the recovered materials in a stock pot, where the values along with traces of base metals would have been cemented. You would then separate all of the solid substances by filtration, or by allowing the solids to settle, then siphoning off the barren solution (the baking soda would have been eliminated by dissolution). You would then incinerate the recovered solids, then start over with nitric. If you discarded any of the solutions you spoke of, they may well have contained values.

Harold

 

[clint s]

hello what i have done so far is i put the material ,i gathered from the stove ,and put it in a big pot then added water let everything settle then poured out the water that was on top, did that for a couple days i notice metals starting to appear more and more as i rinsed the material so i kept rinsing till i had nothing but metals in bottom pot i noticed the more i rinsed the faster it would settle as well , till i had a small amount of metal and everything was rinsed well i took the metal out and put it in a small bottle ,and checked it with 14kt gold testing solution and it did not do nothing so i think it is gold 14 kt a least or the testing solution would of bubbled like crazy ,but before i rinsed it good ,i took some of the cemeted material out and put in crucible and tryed to melt it with my torch got a big chunk melted and ran out of oxygen ,so what i did is put everything that i melted in a solution of nitric and a little h20 and it has been soaking for a day now there is still a lot of metal left in jar but it has been outside and the temperature has been cold here 30 or 40 i will let it sit for another day then filter and rinse then decide if i need to put all the metals i have back in a AR solution again to purify to a better quality .i hope what i melted is gold if so i might have most of the pm back . i have been studying hard on this subject . thanks for your time everything you tell me i listen i have a lot of silver to refine as well hope it goes better, first i need to study more .

thanks Clint

 

[butcher]

Normal glass jars will not take heating. you will need labglass , I use old coffee pots they hold up well if atention is paid to thermal shock.

in hokes book when she said boil, I believe she was talking about slow evaporation (they used steam baths that would not get hot enough to actually boil Aqua Regia, the term boil has been used too loosly in this field by us and others, this use of terms is where alot of trouble begins, these forum discussions help us to change our misuse of these terms.

If you have Karat gold melt with silver quartering it, remove base metals in nitric acid 35%, before trying to dissolve in Aqua regia.

I suggest puting the gold down, the chemicals down, grab something to drink, and a good book, HOKE'S, before your wife rips your eye's out, or worse, you will get farther faster in this field by slowing down and studying than from jumping in to acids with both feet.