hosef
Active member
Cool, that means that I could have zero fumes and collect back as much of the nitric as possible.
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Bullion.Forum
Non-Chemical Keeping the Genie in the bottle. (controling the BFRC)
- Thread starter qst42know
- Start date
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qst42know
Well-known member
hosef said:
That would be very similar to the #3 No Air Dilution scrubber GSP described in this post. Though it uses solid materials for neutralizing.
http://goldrefiningforum.com/phpBB3/viewtopic.php?t=4284&start=0&postdays=0&postorder=asc&highlight=
In small scale I don't know how much pressure the vapors can produce to push through a fluid. Tightly sealed would be even more critical. And you may have to pull it through with some type of vacuum pump to keep it bubbling.
A
Anonymous
Guest
Once upon a time for lack of investment capital to purchase Pyrex glassware, I built a reflux condensation reaction system to process organic reactions... The apparatus can be adapted for aqua regia dissolution, then, modified for distillation and recovery of nitric acid with no toxic discharge into the atmosphere...
I originally planned to provide instructions only for the condenser... But my detail oriented system design mentality took over, causing me to put on my chemical engineer hat and delve into the reflux condensation reaction system, finally leading me to providing operating instructions with an emphasis on safety... I'm posting this to the discussion of condensation and evaporation as applied to the aqua regia process...
In the spirit of Hoke, I hope my composition is understood by the non chemist...
PARTS:
From Tri-Ess Science Supply in beautiful downtown Burbank...
1- 20mm X 48" Pyrex tube ... $6.00 ... (will make two condensers and 60 degree distillation insert)
1 - 1 liter Kymax - Erlenmeyer flask $9.50
1- Rubber stopper - w/20mm hole ... $2.00
From Home Depot
10 ft - 10 mm inside diameter plastic tubing ...$4.00
2 - 8/10 mm Teflon wedge fittings ... $1.50 each
1 - Tube kitchen/bath silicon caulk ... $3.50
1 - Evaporative cooler pump ... $ 16.00 (optional)
From beverage supplier
1 - 2 liter plastic Dr. Pepper bottle $1.00 plus CRV (California Redemption Value)
From Salvation Army store
1 - Used hotplate - $2.50
Assembly instructions...
-Drink Dr. Pepper and rinse bottle...
- Insert 20 mm Pyrex tube through rubber stopper so end is flush with the neck- bottom of Erlenmeyer flask when stopper is inserted... Approximately 1" below the stopper...
-Cut 20 mm hole in bottom of soda bottle, insert tubing in top of soda bottle through 20 mm hole... Bottle will be mounted up-side-down... Allow 4" - 6" between top of stopper and condenser bottle... Scratch Pyrex tube with glass cutter, 4" above inverted bottle... Remove tube from bottle... Support the tube horizontally on both sides of scratch...Tap the scratch from the bottom with metal end of glass cutter while turning the tube... As the tube is tapped, you will see a crack develop... Tap at the end of the crack and follow it around the tube until it snaps in two pieces... Or cut tube with tile saw...Fire polish with propane or Mapp gas…
Cut holes for Teflon wedge connector in side of soda bottle 2" above the neck and 1 " below the (inverted) bottom… Insert wedge fittings and seal with silicon caulk
Insert Pyrex tube through bottle and seal with silicon caulk... Allow 24 hours for curing...
To supply water to the condenser, the 10 mm intake tube can be connected to a water faucet in a sink and discharged directly into the sink drain or attached to a garden hose and diverted to the tomato patch…
For a portable water supply, attach 10 mm plastic tube from lower wedge connection to a 600 cfm (cubic feet/minute) evaporative cooler pump secured in the upper part of a 5 gallon bucket ... Attach another 10 mm plastic tube from discharge wedge fitting into bottom of bucket to re-circulate the water...
Water circulates from pump, securely submersed at top of 5 gallon bucket, to lower intake, fills the condenser and discharges at the top, passes through tubing to bottom of bucket...
To mount the condenser independent of Erlenmeyer reaction flask I drilled a 20 mm hole through the ends of two - 2"X 2" X 24" - pieces of pine... Supports are mounted above and below the condenser, then clamped or bolted to a well anchored shelf unit or work table...
I can't overstress the critical importance of pre-testing the condenser while it is mounted independent of the reaction vessel... Fill the 5-gallon bucket with cold water, activate the pump and watch for leaks...
The condenser will supply adequate cooling for up to a twenty liter reaction vessel... In the portable system, the coolant water gradually heats up... The coolant can be changed periodically simply by moving the discharge tube into an empty bucket or diverted to the tomato patch while adding cold water from a garden hose...
For reactions that use organic solvents, like alcohol or benzene, the Pyrex tube can remain open at the top without losing solvent by evaporation... For acidic solutions, I recommend capping the top of the condenser to avoid losing acid vapor... Or attaching a 20 mm plastic tube at the top and submersing the other end in a water collection vessel...
Nitrogen oxide, NO, is a corrosive gas compressed into a pressure vessel... Nitric acid, HNO3, is nitrogen oxide dissolved in hydrogen dioxide H20 (water)... The balanced chemical equation is NO + H2O = HNO3 ...
When a solution containing HNO3 is heated, the gas, NO is released by evaporation... The reflux condensation system enables one to boil the solution in the reaction vessel, the Erlenmeyer flask... The vapor rises in the condenser tube that protrudes through cold water that circulates through the 2 liter pop bottle condenser... The cold water on the outside of the Pyrex tube causes the acid vapor to condense and drip down to return into the reaction vessel... It’s like an artificial thunderstorm...
When the condenser test is complete, there are no leaks and the condenser, pump, intake and discharge tubes are securely mounted, I recommend testing the system with the reaction vessel filled with plain water... Boil the water by heating over the hot plate... Run the system and monitor the coolant water temperature to get an idea of how often the coolant water must be replaced... Smaller vessels at moderate temperatures (150* to 180 * F.) should run an hour before needing to be cooled ... If you have access to ice, you can cool the water quite rapidly... The reaction flask must be securely mounted independent of hot plate and independent of the condenser, so the hot plate can be removed, the flask disconnected and lowered away from the stopper which enables filling or removing the solution...
If you haven't operated a reflux condensation reaction, you should run the system two or three times so you become familiar with the mechanics... For me, designing, building and operating chemical systems is just as exciting as completing a pure product... I've had my share of surprises, a tube separates causing coolant to spew on a hot plate, or a crucible of molten metal slips from the tongs causing me to jump and dance to avoid shoes full of molten metal and a 911 emergency… My tiny research lab is located in the garage… Beside the garage I have a 2.5 cubic foot natural gas pottery kiln – 2350* F. It sits beside a 3 crucible capacity smelting furnace built in December 2008 – tested to 2400* F.
My home is located between two hospitals with 24 hour emergency service… 5/8ths mile each direction… Think about what you are doing before hand and set up the essential equipment so you can safely shut down a reaction... My first and only serious industrial accident occurred in the same garage while I attended high school in 1968… Summer field science/ chemistry, biology and geology…
Fellow student develops cool contact bombs and graciously shares technology – .25 gram potassium permanganate / .25 g red phosphorous wrapped with a few BB sized granite pebbles in 2” X 2” aluminum foil, the size of a cherry bomb… Device explodes with nice flash-bang when hurled at the ground or a wall…
Dr. Glazo decides to expand the experiment off campus… He correctly theorizes a bigger bang can be obtained by adding .25 g potassium chlorate… He mixes the first test bomb in garage (95* F)… Holding the piece of aluminum foil in one hand, he adds ingredients with metal spoon, only to discover the addition of potassium chlorate oxidizes at 85* F… Mixture detonates causing 2nd degree burns on both palms… Enough said… Impressive learning experience…
The condenser can be remounted to slope down for distillation... A 6" - 8" length of Pyrex is bent in the middle with Mapp gas torch to a 60 degree angle, annealed properly, then, inserted between the reaction vessel top and the end of the condenser tube... When the AR solution is boiled, the nitric acid condenses as it rolls down the slope through the condenser tube and collected in a suitable glass container...
With care and caution, this simple apparatus should provide years of service for AR reactions and subsequent distillation...
I'm going to post before catching a few winks... I'll probably modify and update before posting in the equipment category... I look forward to comments, questions and hopefully constructive critique...
Dr. Glazo... 8) 8)
I originally planned to provide instructions only for the condenser... But my detail oriented system design mentality took over, causing me to put on my chemical engineer hat and delve into the reflux condensation reaction system, finally leading me to providing operating instructions with an emphasis on safety... I'm posting this to the discussion of condensation and evaporation as applied to the aqua regia process...
In the spirit of Hoke, I hope my composition is understood by the non chemist...
PARTS:
From Tri-Ess Science Supply in beautiful downtown Burbank...
1- 20mm X 48" Pyrex tube ... $6.00 ... (will make two condensers and 60 degree distillation insert)
1 - 1 liter Kymax - Erlenmeyer flask $9.50
1- Rubber stopper - w/20mm hole ... $2.00
From Home Depot
10 ft - 10 mm inside diameter plastic tubing ...$4.00
2 - 8/10 mm Teflon wedge fittings ... $1.50 each
1 - Tube kitchen/bath silicon caulk ... $3.50
1 - Evaporative cooler pump ... $ 16.00 (optional)
From beverage supplier
1 - 2 liter plastic Dr. Pepper bottle $1.00 plus CRV (California Redemption Value)
From Salvation Army store
1 - Used hotplate - $2.50
Assembly instructions...
-Drink Dr. Pepper and rinse bottle...
- Insert 20 mm Pyrex tube through rubber stopper so end is flush with the neck- bottom of Erlenmeyer flask when stopper is inserted... Approximately 1" below the stopper...
-Cut 20 mm hole in bottom of soda bottle, insert tubing in top of soda bottle through 20 mm hole... Bottle will be mounted up-side-down... Allow 4" - 6" between top of stopper and condenser bottle... Scratch Pyrex tube with glass cutter, 4" above inverted bottle... Remove tube from bottle... Support the tube horizontally on both sides of scratch...Tap the scratch from the bottom with metal end of glass cutter while turning the tube... As the tube is tapped, you will see a crack develop... Tap at the end of the crack and follow it around the tube until it snaps in two pieces... Or cut tube with tile saw...Fire polish with propane or Mapp gas…
Cut holes for Teflon wedge connector in side of soda bottle 2" above the neck and 1 " below the (inverted) bottom… Insert wedge fittings and seal with silicon caulk
Insert Pyrex tube through bottle and seal with silicon caulk... Allow 24 hours for curing...
To supply water to the condenser, the 10 mm intake tube can be connected to a water faucet in a sink and discharged directly into the sink drain or attached to a garden hose and diverted to the tomato patch…
For a portable water supply, attach 10 mm plastic tube from lower wedge connection to a 600 cfm (cubic feet/minute) evaporative cooler pump secured in the upper part of a 5 gallon bucket ... Attach another 10 mm plastic tube from discharge wedge fitting into bottom of bucket to re-circulate the water...
Water circulates from pump, securely submersed at top of 5 gallon bucket, to lower intake, fills the condenser and discharges at the top, passes through tubing to bottom of bucket...
To mount the condenser independent of Erlenmeyer reaction flask I drilled a 20 mm hole through the ends of two - 2"X 2" X 24" - pieces of pine... Supports are mounted above and below the condenser, then clamped or bolted to a well anchored shelf unit or work table...
I can't overstress the critical importance of pre-testing the condenser while it is mounted independent of the reaction vessel... Fill the 5-gallon bucket with cold water, activate the pump and watch for leaks...
The condenser will supply adequate cooling for up to a twenty liter reaction vessel... In the portable system, the coolant water gradually heats up... The coolant can be changed periodically simply by moving the discharge tube into an empty bucket or diverted to the tomato patch while adding cold water from a garden hose...
For reactions that use organic solvents, like alcohol or benzene, the Pyrex tube can remain open at the top without losing solvent by evaporation... For acidic solutions, I recommend capping the top of the condenser to avoid losing acid vapor... Or attaching a 20 mm plastic tube at the top and submersing the other end in a water collection vessel...
Nitrogen oxide, NO, is a corrosive gas compressed into a pressure vessel... Nitric acid, HNO3, is nitrogen oxide dissolved in hydrogen dioxide H20 (water)... The balanced chemical equation is NO + H2O = HNO3 ...
When a solution containing HNO3 is heated, the gas, NO is released by evaporation... The reflux condensation system enables one to boil the solution in the reaction vessel, the Erlenmeyer flask... The vapor rises in the condenser tube that protrudes through cold water that circulates through the 2 liter pop bottle condenser... The cold water on the outside of the Pyrex tube causes the acid vapor to condense and drip down to return into the reaction vessel... It’s like an artificial thunderstorm...
When the condenser test is complete, there are no leaks and the condenser, pump, intake and discharge tubes are securely mounted, I recommend testing the system with the reaction vessel filled with plain water... Boil the water by heating over the hot plate... Run the system and monitor the coolant water temperature to get an idea of how often the coolant water must be replaced... Smaller vessels at moderate temperatures (150* to 180 * F.) should run an hour before needing to be cooled ... If you have access to ice, you can cool the water quite rapidly... The reaction flask must be securely mounted independent of hot plate and independent of the condenser, so the hot plate can be removed, the flask disconnected and lowered away from the stopper which enables filling or removing the solution...
If you haven't operated a reflux condensation reaction, you should run the system two or three times so you become familiar with the mechanics... For me, designing, building and operating chemical systems is just as exciting as completing a pure product... I've had my share of surprises, a tube separates causing coolant to spew on a hot plate, or a crucible of molten metal slips from the tongs causing me to jump and dance to avoid shoes full of molten metal and a 911 emergency… My tiny research lab is located in the garage… Beside the garage I have a 2.5 cubic foot natural gas pottery kiln – 2350* F. It sits beside a 3 crucible capacity smelting furnace built in December 2008 – tested to 2400* F.
My home is located between two hospitals with 24 hour emergency service… 5/8ths mile each direction… Think about what you are doing before hand and set up the essential equipment so you can safely shut down a reaction... My first and only serious industrial accident occurred in the same garage while I attended high school in 1968… Summer field science/ chemistry, biology and geology…
Fellow student develops cool contact bombs and graciously shares technology – .25 gram potassium permanganate / .25 g red phosphorous wrapped with a few BB sized granite pebbles in 2” X 2” aluminum foil, the size of a cherry bomb… Device explodes with nice flash-bang when hurled at the ground or a wall…
Dr. Glazo decides to expand the experiment off campus… He correctly theorizes a bigger bang can be obtained by adding .25 g potassium chlorate… He mixes the first test bomb in garage (95* F)… Holding the piece of aluminum foil in one hand, he adds ingredients with metal spoon, only to discover the addition of potassium chlorate oxidizes at 85* F… Mixture detonates causing 2nd degree burns on both palms… Enough said… Impressive learning experience…
The condenser can be remounted to slope down for distillation... A 6" - 8" length of Pyrex is bent in the middle with Mapp gas torch to a 60 degree angle, annealed properly, then, inserted between the reaction vessel top and the end of the condenser tube... When the AR solution is boiled, the nitric acid condenses as it rolls down the slope through the condenser tube and collected in a suitable glass container...
With care and caution, this simple apparatus should provide years of service for AR reactions and subsequent distillation...
I'm going to post before catching a few winks... I'll probably modify and update before posting in the equipment category... I look forward to comments, questions and hopefully constructive critique...
Dr. Glazo... 8) 8)
yvonbug
Well-known member
All the idea's and info in this one thread! You guys are all great. The reading of all this info is more fun than, uh, well, it's lots of fun! Anyways, I think I'll try the inverted soda bottle with the marbles. I don't really need too much as I'm out here in the sticks. And that seems to be easy and quick. I mainly just worry that my goat will get too much a wiff of the stuff. I can't stand it, why should he? Thanks again guys! You make it fun as well as safe for us backyard refiners! -Yvonne-
