You are on page 1of 4

Procedure for Reclaiming Heavy Liquids AGES Lab Below are the steps we use to reclaim MEI and

LST after using it to separate out specific minerals. These are not the only ways to separate out these liquids, however, after trying multiple methods, we have found these to be the best. Feel free to contact us with any questions (epierce@ldeo.columbia.edu, mesko@ldeo.columbia.edu ). MEI Reclaiming Process Below are steps that should be followed in order to reclaim MEI from the MEI/Acetone mixture that is produced when performing heavy mineral separations. Since water is immiscible in MEI, and since acetone dissolves in water, adding water to the MEI/Acetone solution will cause the acetone to dissolve in the water, and to float to the top. You will need: Separatory funnel (500 mL, or 1000 mL if possible); stopcock; ring stand to hold funnel; rubber stop for top of funnel, squirt bottle of acetone; small (200 mL) glass beaker for collecting clean MEI; small (200 mL) beaker for collecting the MEI/water+acetone interface; large (1000 mL) beaker for pouring MEI/Acetone mixture into the separatory funnel; large (1000 mL) beaker for pouring DI water into the separtory funnel; plenty of DI water; a glass stir rod; container to place reclaimed MEI in; hydrometer for testing density of reclaimed MEI; waste container for the acetone/water solution (should be labeled as 80% water, 20% Acetone, <1% Methylene Iodide) All of the following steps must take place inside the fume hood, and you must wear long gloves. MEI is toxic and therefore should not be inhaled, and skin contact must be avoided. All kimwipes and gloves used in the process are stored in one of the blue garbage bags under the Frantz for special waste pickup) 1. Set up your separatory funnel with the ring-stand; make sure that funnel is at a height so that you can comfortably pour solutions into the top; put the stopcock in. (You may use a glass funnel to facilitate pouring into the separatory funnel, however this will make it harder as you have now increased the pouring height a few inches).

2. Label your beakers (according to sizings above) as Clean MEI, DI water, MEI/Acetone for Reclaiming, Acetone + Water. 3. Pour ~200 mL (400 mL if using a 1000mL funnel) of the MEI/Acetone solution into the appropriate beaker. Ensure that the stopcock is in the closed position. Pour the solution into the top of the separatory funnel. Do NOT place your Clean MEI beaker under the funnel in case you spill any of the mixture while pouring. 4. Pour some DI water into a beaker. Use this beaker to then pour DI water into the funnel; this will stir the up the MEI/Acetone solution. Fill the funnel, and use a glass stirring rod to further mix the two solutions. 5. Rinse the stirring rod with acetone into the MEI/Acetone for Reclaiming beaker and dry with a Kimwipe. Place the rubber plug in the top of the funnel. 6. Allow for ~ 20-30 minutes for separation of the MEI from the Acetone/Water. The MEI should be clear when the separation is complete (not cloudy). 7. Once the solutions have separated, you will empty the funnel in 3 steps. It is important to keep the rubber stopper in the top of the funnel for the first two steps, as it keeps the flow rate to a minimum: a. Place the clean MEI beaker under the funnel. Open the stopcock and allow the clean MEI to flow until you are close to the MEI/Acetone+water interface (~ when there is MEI only in the narrow tip of the funnel above the stopcock). Then stop the flow. Pour the clean MEI into the appropriate container. b. Place the MEI + Water/Acetone beaker under the funnel. Open the stopcock and allow to flow until the MEI and the first of the Water/Acetone mixture has been emptied. Pour this into the MEI/Acetone for Reclaiming beaker (this will be processed again in the next step; by doing this we only loose that interface of MEI and Water/Acetone in the very last step). c. Place the water and acetone beaker under the funnel and now drain the funnel, with the rubber stopper now removed. You will have to lift the funnel at the end so that it is not sitting in the waste solution. Remove the beaker from the stand; close the stopcock; pour the acetone/water solution into the waste container. 8. You are now ready to repeat steps 1 through 7. Do this until you have reclaimed all of your MEI.

9. Now test the density of your MEI. MEI is generated with a density of 3.32 g/cc. We use this for separating zircons (4.6 g/cc) from apatite (3.22 g/cc). A minimum density of 3.3 g/cc is allowed. If your MEI is not dense enough, there is still acetone in the mixture, and you will have to reprocess all of the MEI again. 10. Once finished, all glassware must be cleaned; anything that had even trace amounts of MEI in it must be rinsed with acetone; put these washings into one of the MEI/Acetone for Reclaiming containers you just emptied. This MEI will be processed next time.

LST Reclaiming Process Below are steps that should be followed in order to reclaim LST of appropriate density from the dilute LST waste water that is produced when performing mineral density separations. LST contains hydrated crystals of lithium heteropolytungstates. Wear goggles to avoid contact with eyes. You will need: 2000mL filter flask; 2000mL beaker; vacuum pump, vacuum tube; drying oven; 100mL graduated cylinder; stirring rod; deionized water; bottle for storing reclaimed LST; precision hydrometer suitable for heavy liquids; nitrocellulose membrane filter paper (0.22m GS); and a glass vacuum filtration assembly consisting of: glass funnel top, glass frit base, clamp, and appropriately-sized rubber stopper with hole large enough to accommodate the tube on the glass frit. (See image) 1. 2. 3. 4. Funnel Clamp Base (glass frit) Rubber stopper

1. Connect your 2000mL filter flask to your vacuum pump using the vacuum tube. This will initially store your filtered LST. Set the glass vacuum filtration assembly on top of the filter flask. Next,

2. 3.

4.

5. 6.

7. 8.

place a sheet of nitrocellulose membrane filter paper between the funnel and glass frit. Clamp securely in place. Pour the unfiltered LST solution into the funnel. Then, start the vacuum pump. Filtered LST will now begin collect in the flask. Continue to add unfiltered LST to funnel while monitoring the filter paper. Filter paper will have to be replaced about as frequently as once per every 1 and funnel fills. The filter paper will start to turn tan and the flow of LST will slow when paper needs to be replaced. Turn off vacuum pump before replacing the filter paper. Once a suitable amount of filtered LST has been collected, shut off the vacuum pump. Pour the filtered LST into the 2000mL beaker. Label it filtered LST. Then, place the beaker in the drying oven to evaporate off the excess water. You will want to evaporate the LST down to a density greater than your target density, so you will then be able to add deionized water in small increments to dilute the LST to the proper density. If crystals are forming in the warm solution, then the LST is saturated and too much water has been evaporated off. Once you have evaporated off the excess water, remove the beaker from the drying oven and allow the LST to cool to room temperature. Fill your 100mL graduated cylinder to about 100mL. Use the precision hydrometer to measure the density of the LST in the graduated cylinder. Then, pour that LST back into the beaker. Add a small increment of water to your LST. Stir vigorously for a few minutes until the solution is well-mixed. Repeat step 6 until you reach your desired LST density, like 2.85g/mL or 2.64g/mL. If you overshoot your desired density, place the beaker back into the drying oven and start back at step 5. Finally, with your LST reclaimed at your desired density, pour it into your bottle labeled with the achieved density for storage at room temperature.

Related Interests