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Standard Operating Procedure
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Print out the completed SOP and keep a readily accessible hard copy in the lab
(also keeping an electronic copy is highly recommended).
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Date:
SOP Title:
Solvent Still usage
Principal Investigator:
Room and Building:
Lab Phone Number:
Section 1 – Process
Solvent distillation/ purification Quenching of drying agents.
Section 2 – Hazardous Chemicals
Tetrahydrofuran, methylene chloride, acetonitrile, triethylamine, pyridine, organic solvents, calcium
hydride.
Section 3 – Potential Hazards
Tetrahydrofuran is flammable, irritant, and can form peroxides. Methylene chloride is notflammable
but is harmful, and probable human carcinogen. Pyridine is flammable and harmful. Acetonitrile is
flammable and harmful. Triethylamine is flammable and corrosive. Calcium hydride is flammable
and reacts with moist air (pyrophoric). Review MSDS if not familiar with hazards of these chemicals.
Section 4 – Approvals Required
New students as well as researchers who are not members of the lab are required to undergo
training on how to operate the stills safely.
Section 5 – Designated Area
There is a fume hood dedicated to the solvent stills.
Section 6 – Special Handling Procedures and Storage
Requirements
Running cold water and nitrogen flow are requirements. Temperature controls should not be turned
beyond the indicated markings that are solvent specific. Never use alkali metals to dry chlorinated
solvents. Make sure not to distill any flasks to dryness because peroxide can become concentrated
and be explosive.
Section 7 – Personal Protective Equipment
Gloves, fire resistant lab coat, and safety glasses should be worn when using the solvent stills.
Section 8 – Engineering/Ventilation Controls
The solvent stills should always been kept within the fume hood and the sash drawn down when not
in use.
Section 9 – Spill and Accident Procedures
If there is a spill into sanitary sewer, call the number posted on top of all the sink drains. For minor spills, spill kits
can be. For exposure to solvents, use eye wash and safety shower are by the north door. Fire extinguisher can be
found in the hallway. If injured by shattered glassware, contact the Tang center – telephone numbers are on the
refrigerator in the group room. For large scale spills, evacuate the room and call EHS.
Section 10 – Waste Disposal
For chemical solvent disposal, follow general EHS disposal guidelines. Quenching of the stills must
always take place in a fume hood. Remove any potentially flammable materials from the vicinity.
First, cool the still pot to room temperature. Cool it further in an ice water bath. Begin the quenching
procedure by slowly adding isopropanol to the still pot. Ensure proper ventilation since gas will
slowly evolve. Let it sit for about 12 hrs., or until gas has stopped evolving. Progress ethanol, then
methanol, and finally water. After each step, allow 12 hrs. between each step or until no more gas
has stopped evolving. Dispose of the liquid in the hazardous waste disposal.
Section 11 - Decontamination
Use spill kit where necessary, and use safety shower.
Section 12 – Process Steps
This section is useful for particularly complex or multi-step processes. List each step of
the process or procedure chronologically on the left side of the SOP Template page.
On the right side of the page and directly across from the corresponding process steps,
list precautionary safety measures to be taken, including the use of specific laboratory
techniques and PPE. If possible, describe indicators (visual or otherwise) which show
whether the reaction, equipment, etc. is working safely as intended or that a hazardous
situation may be developing.
Process Steps
Turn on water.
Turn on temperature control to the designated
setting.
Start collecting solvent in the upper bulb.
Use needle to extract solvent.
Turn off temperature control when done. Wait
for solvent to cool down.
Make sure to turn off water.
Safety Measures
Make sure water flow is just enough, without
causing the water level to spill over.
If still is dry, do not turn on the temperature.
Make sure never to turn the temperature setting
above the designated marking.
Make sure valve isn’t leaking and solvent does
not condense past condenser.
Be careful with sharp needle. Keep needle
capped when not in use. Use proper syringe
technique to avoid overdrawing solvents.
Training Documentation
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