Standard Operating Procedure

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Read the EH&S Standard Operating Procedures Fact Sheet before filling out this form. Print out the completed form 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: November 8, 2010 Distillation Richmond Sarpong 841 Latimer (510) 643-2485

Principal Investigator: Room and Building: Lab Phone Number:

Section 1 Process
Distillation Equipment: Microdistil, normal distil, Vigreux-column, Kugelrohr-distil, vacuum pumps, cooling traps

Section 2 Hazardous Chemicals

A Job Hazard Assessment should be performed for work involving distillations of organic liquids and should thoroughly address the potential combination of water and electricity (shock hazards), the temperature and temperature control of the heating mantle and contents (burn and fire hazards), chemical toxicity and reactivity of the solvents and sodium reducing agent, cleanup and disposal of still pot residue, solvent storage, and required Personal Protective Equipment (PPE).

Section 3 Potential Hazards

Contact with hot parts can lead to burns. Never distil in a closed system; always allow for pressure exchange to atmosphere, nitrogen line or Vacuum, as overpressure could potentially lead to explosions. If cooling water is used, secure tubing with clamp; make sure the outlet is in the sink. Evaluate if there is a potential for an exothermic reaction like explosion of peroxides or other High-energy compounds (e.g. nitro-compounds, epoxides, acetylenes). If so, try to avoid the distillation, or use a blast shield. Never set glassware with a crack under vacuum as it may implode.

Section 4 Approvals Required

See the lab mate assigned for this job for specific training and references.

Section 5 Designated Area

Fume hood, except for Kugelrohr-distil, which has its own splatter protection and may be used outside the hood.

Section 6 Special Handling Procedures and Storage Requirements

See Section 12.

Section 7 Personal Protective Equipment

Same as for any lab-work. Keep fume hood closed as much as possible.

Section 8 Engineering/Ventilation Controls

Work in fume-hood

Section 9 Spill and Accident Procedures

If glass breaks keep in mind that it may be sharp. If joints are stuck always wear leather gloves while trying to set them free.

Section 10 Waste Disposal

Depends on chemicals used. See laboratory procedures.

Section 11 - Decontamination
Depends on chemicals used. See MSDS sheet for chemical in question.

Section 12 Process Steps

General distillation equipment consists of the following glass parts: Kugelrohr distil; high vacuum oil pump (ca. 0.1 mbar); medium vacuum membrane pump with vacuum controller (5-1000 mbar). Use the sign-out book if you take any part to your personal bench or hood. Notify the responsible person if any part is broken or missing.

Always use a cooling trap when using one of these two pumps. When using the high-vac pump, please remove residual solvent under high vacuum in your line to further minimize the amount of volatiles that could potentially go into the pump and deteriorate the quality of the vacuum. Microdistil: For volumes of a few to ca. 50 ml Normal distil: For volumes above ca. 10 ml. This equipment requires two clamps, one to hold the flask that is in the oil bath and one that holds the collection bulb. A lab-jack with cork ring may replace the second clamp. Make sure there is no tension which could cause the glass to break.

Kugelrohr-distil: For volumes from 0.2 ml to ca. 10 ml. Advantages: Simple and fast set-up, fractional distillation in one step possible, temperatures up to 250 C possible. Immediately after use, clean with acetone, as high-boiling compounds can diffuse into rubber seals and cause them to swell and subsequently leak. Choosing the right vacuum pump: Membrane-pump: Goes down to ca. 5 mbar (boiling point at normal pressure <200 C) Vacuum line pump: is generally at 0.5-2 mbar High-vacuum pump: gives at least 0.1 mbar, or better on good days.

Training Documentation
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