Flask failed, mantle mess

[Noggin]

Hi all, I have values (salts and metals) tied up in the kaowool insulation after a flask failure.
Tests on the kaowoll indicate:
1. Heating kaowoll with metal on it did not produce a bead
2. Rinsing in water gets some out but also ties up more in the loose fibers.

There’s a decent amount of platinum and palladium in there (some in salts that survived, I believe) and maybe some small amounts of gold.

My only real idea is:
1. Rinse out what I can and save the kaowool
2. Pre-mix some of my AR and pour it through some of the wool during future refinings till it’s clean.

I was distilling to concentrate prior to precipitation when the flask broke.

Here are some pictures for your amusement. The last few shows the results of my rinsing and wringing test.

Root cause was I was in a hurry and had the heat high enough to boil over into my receiver. I cleaned up the receiver and condenser, and put the liquid back in not realizing the vessel was broken.

Please let me know if you have any chemical/mechanical solutions, thanks!!

 

[Elemental]

Sorry for the loss, my first thought would be to take the contaminated Kaowool and use AR to soak it to re-dissolve your PM's back into solution, followed by a thorough rinsing/filtering of the Kaowool afterwards. (Basically let the aqua regia do the work of getting your PM's out of the wool) Hopefully someone here can give you a better idea on how to recover from this. Please be careful dealing with the platinum salts, as they are quite toxic and can be absorbed through the skin.

 

[Noggin]

Thank you Elemental

Ref platinum salts, I appreciate that warning. You might be able to tell from the pictures, I'm doing this in my fume hood (which I completely cleaned with HCL and then put the paper towels in a covered 5 gal bucket with the rest of the carnage). I am proceeding carefully, testing each possible solution on a small bit of waste.

As you suggest, I might try putting some kaowool in a funnel and pour AR through, like it was a rolled cotton filter and see how that cleans it up. I can imagine it's going to take a while to fix this since I think I need to use virgin AR. Would you try to convert the salts to metal at this time, so there is only metal in the kaowool?

 

[Elemental]

I would propose you put some of the contaminated wool in a large beaker, add your HCL and then slowly add nitric acid in small increments to make your AR. (I personally would not try your filter idea. AR in motion is risky and it might take several passes of it to dissolve the salts. You are not worried about the wool, although I’m not sure if AR will put the minerals from it in solution. Even if it did, cementing with copper will drop the PMs.) This would put your metals into solution, which you could cement out after filtering.

I would start with a small test as well to see how the recovery looks and then scale/batch from there. I’m assuming you are trying to separate the platinum, palladium, and gold? What I am proposing doesn’t help with that and is more concerned with recovery at this point.

I will caveat that I’ve not done PGM separations yet and this is purely from a chemistry background sort of suggestion. You would be wise to seek advice from some of the seniors here with more experience than I. I am glad you are aware of and managing the PGM salt risks.

Also, look at the solubility of your salts. They may dissolve easier in water (or a different solvent) only, then you could look at AR for the metal recovery. Hope this helps.

Final note: Don’t rush this. The values are still there, try to figure out the best recovery option and go from there.

Elemental

 

[Elemental]

Noggin,

Any updates on how your recovery went? Any advice or wisdom learned?

Elemental

 

[Noggin]

Noggin,

Any updates on how your recovery went? Any advice or wisdom learned?

Elemental

Hi Elemental,
I’ve manually picked off the chunky stuff from the mantle and broken flask and recovered over 20 grams just with that. I’m missing about 30 grams from this batch but with over a kilo of gold filled I could be off. Due to medical issues with the wife I’ve had some delays but the Christmas holiday break should let me catch up. So here’s the plan:

1. Wash soluble salts off in hot water. Cement with copper and refine.
2. Drop kaowool in AP (peroxide 40%) till solids are dissolved. Pull solution through fritted funnel and add rinse water. Repeat till AP remains clear.
I will use AR on the residue and test for platinum and palladium.
I may add a distillation step to recycle unused AP and concentrate the gold for a better drop (I have a low-waste setup so I do this anyway).
I still need to process the paper towels I used to clean up. There’s a decent amount in there.
I’d love your feedback or tips!
I might publish a video if it gets interesting.

 

[Elemental]

Noggin,

I'm glad to hear you've recovered over 40% of your distillation. Hopefully you manage to pull quite a bit more from the paper towels. More importantly, I'm sorry to hear about the medical issues with your wife. I hope she manages a quick recovery.

I'm glad to hear that AP is working out well with the Kaowool. I was worried that it might complicate things. I think by treating each component of the recovery separately, you'll increase your percentage of recovery. Your plan above looks solid, just ensure you do plenty of testing with Stannous to ensure your solutions are void of any PGM, and you'll be alright.

If you do manage to video it, I look forward to seeing it, along with your final results. I suppose my final question for you would be how would you prevent this from happening again? How could you have put a secondary containment between your mantle and flask or sealed your mantle so your solution would just pool in the bottom?

Elemental

 

[Noggin]

Noggin,

I'm glad to hear you've recovered over 40% of your distillation. Hopefully you manage to pull quite a bit more from the paper towels. More importantly, I'm sorry to hear about the medical issues with your wife. I hope she manages a quick recovery.

I'm glad to hear that AP is working out well with the Kaowool. I was worried that it might complicate things. I think by treating each component of the recovery separately, you'll increase your percentage of recovery. Your plan above looks solid, just ensure you do plenty of testing with Stannous to ensure your solutions are void of any PGM, and you'll be alright.

If you do manage to video it, I look forward to seeing it, along with your final results. I suppose my final question for you would be how would you prevent this from happening again? How could you have put a secondary containment between your mantle and flask or sealed your mantle so your solution would just pool in the bottom?

Elemental

Hi, thanks for the feedback and encouragement.
Unfortunately a 1000ml boiling flask fits a standard uniform heating mantle. Here's the Y chain:
Problem: Boiling flask breaks, day is ruined.
Why? Likely overheating due to dry flask.
Why? Found all liquid in receiving vessel so heat was too high (I poured this back in after cooling it a bit, not realizing it was broken)
Why? I bought a cheap mantle without a digital temperature setting.
My next mantle will have a temperature setting and probe. These are way more expensive. Also I ran the distillation (removing nitric and water from sulfuric slurry) successfully with my hot plate last week so it's not an emergency but it takes much longer.
I'll let you know when I get the video up. Merry Christmas!

 

[butcher]

A heated vessel builds pressure pushing the expanded volatile gases from the distillation flask.

water when heated and when it flashes into steam, the steam will take up 1,700 times the original volume of the water, this builds pressure in a closed vessel (the pressure raises the boiling point of water).

A vacuum or removing the atmospheric pressure from a vessel will lower the boiling point of water.

If cooled this flask is cooled or the temperature is lowered during distillation, the gases will condense lowering their volume within the flask, it will develop a suction (lowering the vessel below atmospheric pressure), and if your setup can suck back cooler liquid into the hot flask, you will break or explode your flask splashing hot acid everywhere.

Study safety if you are attempting to distill. it can be a dangerous operation in a lab if you do not understand its principles or its safety concerns..

 

[Noggin]

A heated vessel builds pressure pushing the expanded volatile gases from the distillation flask.

water when heated and when it flashes into steam, the steam will take up 1,700 times the original volume of the water, this builds pressure in a closed vessel (the pressure raises the boiling point of water).

A vacuum or removing the atmospheric pressure from a vessel will lower the boiling point of water.

If cooled this flask is cooled or the temperature is lowered during distillation, the gases will condense lowering their volume within the flask, it will develop a suction (lower than atmospheric pressure), and if your setup can suck back cooler liguid into the hot flask, you will break or explode your flask splashing hot acid everywhere.

Study safety if you are attempting to distill. it can be a dangerous operation in a lab if you do not understand its principles or its safety concerns..

Thanks Butcher. You just reminded me: I bought a vacuum trap to take advantage of those lower boiling temperatures without ruining my vacuum pump.

It wasn't a pressure break but a temperature shock from running it dry. I'm hoping to be able to distill faster and easier by pulling vacuum. I wish I'd been there for it - even if I didn't avoid the boilover I could have avoided a disaster!

 

[Elemental]

Look at you buying those fancy vacuum traps, I made one with a mason jar and a couple of elbow fittings. (I try not to redneck all my apparatus, but this one was a simple one!)

Definitely need to look for a temperature regulated mantle. I remember using the one you have, that just plug in and get hot. We used to have to stand around pull the power cord when the temperature got too high, wait for it to fall, then plug it back in.

 

[butcher]

I would never distill anything and leave it unattended.

Your glassware should be able to handle a very high temperature even dry.
The problem comes from improper care. or using the wrong type of glassware, using the glassware improperly, uneven heating solids sitting on the bottom of the vessel can lead to this as well as other factors, thermal shock, a fast or drastic change in temperature, scratches or cracks damage, extreme pressure or vacuum above what the ware is designed to handle, well the list goes on.

I have broken a lot of glass, I am sure I will break a few more. and learn even more way's I can break glass and the reasons why glass gets broken.

Catch basin can help contain a mess.