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Reaction flask

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Amazing posts 4metals, as always. Snoman has asked most of the questions that I would have asked.

In the reaction vessels I see that they are closed and have no entry for air. With a vacuum regulator you could control the pressure if the reaction is weak to prevent shattering the reaction vessels but if the reaction is strong (eg atomized materials) how would you control it? The gasses would either push the conical stoppers and leaking starts. I would assume the operator has everything controlled somewhat somehow.

In my small setup, the only way I could get this to work is by replacing the condenser with a bigger one and larger diameter hoses for higher CFM output along with a small entry for air in the reaction vessel. Before I was having problems with the condenser not even working because the vacuum pressure was too high that it was already pulling the liquid it condenses to the scrubber unit.

I was always trying to figure out how to remove the liquid/solids from such big reaction vessels, I always thought that it could have been by inserting a vacuum hose and continuous washing or through a bottom drain. There is no way I am going to lift a 12L vessel full of gold liquid. That is just a risk I cannot afford! Even this 4L flasks that I am working on with right now, I know sooner or later I might bump it somewhere and could end up shattering it. As long as its moving there's a risk. I would either go for that tilting device or a bottom drain.

How about using PP filter cartridges for AR liquids?
How about stirrers? I believe the best reaction vessel should have its contents agitated without breaking the actual vessel.
 
In the reaction vessels I see that they are closed and have no entry for air. With a vacuum regulator you could control the pressure if the reaction is weak to prevent shattering the reaction vessels but if the reaction is strong (eg atomized materials) how would you control it? The gasses would either push the conical stoppers and leaking starts. I would assume the operator has everything controlled somewhat somehow.

The reactor is not closed, the top of the condenser is open to the exhaust ductwork and I have never seen too much pressure build up to pop out the glass stoppers. When processing reactive material with high surface area, the rate of the reaction is controlled by the rate of chemical addition or the feed of the material. One of the benefits of a spherical vessel is as a reaction rises the shape seems to push the rising foam into the center and knock itself down. Of course if you overdo it you can overflow any vessel. These reactors are never filled more than 60% of capacity, so a 12 liter flask will never be filled with more than 7 liters of acid, really not too heavy to manually handle. They even make a 5 liter vessel that takes the same heads, that is lighter and I usually use them for platinum stone removal lots.

The airflow out of these reactors through the condenser is quite low and if you vent it by loosening a glass stopper the flow will increase. If you come in to your shop in the morning after a reaction was run the night before, the fume will be visible in the vessel and the connection to the condenser because there is very little fume escaping even though the condenser is open to the vent. By removing the top glass stopper, the airflow immediately evacuates all of the fume up through the condenser.

How about using PP filter cartridges for AR liquids?

I am not a big fan of poly wound cartridges, they are difficult to rinse free of values and by their very nature they are contained in an opaque cylinder so you cannot keep an eye on the filtration surface. To recover any values they must be incinerated and the ash processed. And they do not exactly burn with a clean smoke free stack.

How about stirrers? I believe the best reaction vessel should have its contents agitated without breaking the actual vessel.

I have used these vessels extensively for karat gold refining and stone removal. With karat gold I always made sure the silver content was as low as possible, never above 9%. This will allow the acid to react and minimize gold trapped in the chlorides without stirring.

As far as diamond removal, never stir the reaction. When I first started doing stone removal chemically, in the early 1980's, I thought stirring would be good. It actually makes good sense because you cannot control the assay so some pieces will have in excess of 9% silver. I learned the hard way that stirring causes the material to move about against the glass. With diamonds this meant they scrape against the glass and scratch it. This weakens the glass and eventually you pick up the vessel and the bottom piece, in the shape of a large watch glass, breaks out. Really quite the mess, destroys the mantle, gold recovery is a nightmare, not something you want to experience.

Processing jewelers sweeps in aqua regia would benefit from a stirrer but I prefer to process sweeps in a titanium bucket and stir with a stir rod.
 
Acids on tap....I like that!

Acid on tap is a real convenience! The drum of acid is stored alongside the hood and connected by tubing. (The tube entering the top of the reservoir in the picture connects to the acid drum.) A vacuum tube connects permanently to the reservoir and when the vacuum is turned on by opening the valve, acid is drawn from the drum into the reservoir. There are no float valves to prevent overfilling as that would be too complicated, instead I added a tee with a cap between the valve and the tubing connecting the vacuum to the jug. There is a cap on the tee with a 3/8" hole drilled in it. When you turn on the vacuum valve it still will not draw acid into the jug. You need to place a finger over the hole to generate suction. When you remove your finger the suction is lost and flow stops immediately. This makes the operator the safety valve because you have to stand there with your finger on the hole. The reservoir has a nice teflon and glass spigot to dispense acid into your measuring container.

I like to set up a 5 gallon reservoir on one end of a tabletop hood for Hydrochloric and a 2 1/2 gallon reservoir on the other end for Nitric.

The feed pipes into the acid drums have a built in water trap to burp under vacuum so the drum doesn't implode and the small moat of water keeps the acid from fuming into the shop.

IMG_2511 - Version 2.JPG
 
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