cally quenched to prepare the still bottoms for disposal. This usually involves adding solvent to consume the scavenging agents. The process itself poses a risk of reactive metal adhering to the bottom of the flask, with the potential for exposure to air, potentially causing a spontaneous fire. Most thermal stills rely on electric heating mantles to heat the flammable solvents upward of 82 °C (180 °F), presenting a fire risk and potential ignition source.

Always set up stills in a chemical hood. Although many procedures suggest allowing the process to run overnight, it is prudent to ensure that it is not left completely unattended. Start the process at the beginning of the day and let it run as long as laboratory workers are present. Place Plexiglas shields around the still to protect workers in the event of a serious accident. Deactivate the stills under argon or nitrogen, never air. Do not add fresh solvent, drying agent, or indicator while the still is hot. Ensure that water cooling lines are in good condition. Do not allow material to accumulate at the bottom of the still; quench the still at the end of every procedure and clean thoroughly. Use caution when collecting the reactive materials as waste.

7.C.6.2 Column Purification Systems or “Push Stills”

Column purification systems offer a safer, more environmentally friendly process for providing dry, oxygen-free, high-purity solvents as compared with thermal distillation. The level of impurity (water, oxygen, peroxides) is comparable to thermal distillation. The system is usually composed of refillable stainless steel “kegs” that hold high-purity solvent and act as a solvent reservoir. Inert gas (nitrogen, argon) is used to maintain an inert atmosphere as well as to force solvent through the packed columns that contain activated alumina (for water scavenging) and copper catalyst (for oxygen scavenging). For those solvents that are incompatible with copper (e.g., tetrahydrofuran, methylene chloride, acetonitrile), a second column of alumnia is used along with a dry nitrogen or argon purge to facilitate oxygen removal. The solvent product is dispensed from the columns into a variety of specialized containers for use in the laboratory (glass, stainless steel, etc.).

Column purification systems (Figure 7.4) present much less of a fire risk compared with thermal distillation, because they do not employ heating devices or reactive metals. Because glass containers are not needed, the potential for injury or spill related to breakage is also eliminated.

The column purification system significantly reduces utility usage compared with a thermal still. Thermal distillation uses an average of 70,000 gal of water per coolant line, per year; the column purification system uses no water. There is no need for heating mantles when solvent is present, and the intrinsically safe properties of the system allow it to be set up virtually anywhere in the laboratory, thus eliminating the need to place the apparatus in a chemical hood. As a result, there is a significant savings in electricity usage, although heating jackets may be required for installations where the water and oxygen scavengers are activated or regenerated.


FIGURE 7.4 Example of a column purification system.

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