6/20 AM
Well, after the jar mills spent the night in a spin cycle, we went through several steps to recover as much product as possible while losing as little
as possible.
First, we poured the slurry (reagants and ethanol) and balls from the bottle in a large, glass petri dish. Much of the slurry had stuck to the sides of the bottle, so we spent considerable time rinsing the inside of the bottle with ethanol, then pouring it out into the petri dish. Unfortunately, not all of the reagent mixture could be removed with an ethanol rinse. It appeared that the solid had leached into the bottle. So after a few attempts and many milliliters of ethanol, the rest of the reagent was given up for lost. The petri dish was then placed in a 120 degree oven to evaporate the ethanol.
Once the ethanol appeared to have completely evaporated (about 20 minutes), there was a considerable amount of reagent stuck to the balls used for milling. One-by-one, we removed the balls with forceps and rinsed them with acetone. The purpose of this was to maximize the amount of product that we could get from the process. Just estimating, there was probably 100 balls to individually pick up with forceps, then rinse and scrape until they were as clean as possible. Unfortunately, this was mostly a feeble effort. Very little of the product came off the balls. It was definitely necessary because leaving product behind is a sin in the lab, but picking up these balls that were less than 1 cm on their longest edge
Once we had given up the balls for a lost cause we put them in a large petri dish, then in the 120 degree oven to evaporate any remaining acetone. Having a sore back from leaning over the counter, and frayed nerves from spending an hour feeling mostly incompetent, we broke for lunch.
Well, after the jar mills spent the night in a spin cycle, we went through several steps to recover as much product as possible while losing as little
as possible.
First, we poured the slurry (reagants and ethanol) and balls from the bottle in a large, glass petri dish. Much of the slurry had stuck to the sides of the bottle, so we spent considerable time rinsing the inside of the bottle with ethanol, then pouring it out into the petri dish. Unfortunately, not all of the reagent mixture could be removed with an ethanol rinse. It appeared that the solid had leached into the bottle. So after a few attempts and many milliliters of ethanol, the rest of the reagent was given up for lost. The petri dish was then placed in a 120 degree oven to evaporate the ethanol.
Once the ethanol appeared to have completely evaporated (about 20 minutes), there was a considerable amount of reagent stuck to the balls used for milling. One-by-one, we removed the balls with forceps and rinsed them with acetone. The purpose of this was to maximize the amount of product that we could get from the process. Just estimating, there was probably 100 balls to individually pick up with forceps, then rinse and scrape until they were as clean as possible. Unfortunately, this was mostly a feeble effort. Very little of the product came off the balls. It was definitely necessary because leaving product behind is a sin in the lab, but picking up these balls that were less than 1 cm on their longest edge
Once we had given up the balls for a lost cause we put them in a large petri dish, then in the 120 degree oven to evaporate any remaining acetone. Having a sore back from leaning over the counter, and frayed nerves from spending an hour feeling mostly incompetent, we broke for lunch.
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