Column Installation and Troubleshooting


Methanol, methylene chloride and hexane are recommended and work very well for the majority of cases. Acetone can be substituted for methylene chloride to avoid using halogenated solvents; however, methylene chloride is one of the best rinsing solvents. If aqueous based samples (e.g., biological fluids and tissues) were injected, use water before the methanol. Some residues originating from aqueous based samples are only soluble in water and not organic solvents.Water and alcohols (e.g., methanol, ethanol, isopropanol) should be used to rinse bonded polyethylene glycol based stationary phases (e.g., DB-WAX, DB-WAXetr, DB-FFAP, HP-Innowax) only as a last resort.


Table 8 lists the suggested solvent volumes for different diameter columns. Using larger solvent volumes is not harmful, but rarely better and merely wasteful. After adding the first solvent, pressurize the rinse kit, but stay below 20 psi. Use the highest pressure that keeps the solvent flow rate below 1 mL/min. Except for most 0.53 mm I.D. columns, the rinse kit pressure will reach 20 psi before the flow rate reaches 1 mL/min. Longer rinse times are required when using heavy or viscous solvents, and for longer or smaller diameter columns. When all or most of the first solvent has entered the column, add the next solvent. The previous solvent does not have to vacate the column before the next solvent is started through the column.


After the last solvent has left the column, allow the pressurizing gas to flow through the column for 5-10 minutes. Install the column in the injector and turn on the carrier gas. Allow the carrier gas to flow through the column for 5-10 minutes. Attach the column to the detector (or leave it unattached if preferred). Using a temperature program starting at 40-50°C, heat the column at 2-3°/min until the upper temperature limit is reached. Maintain this temperature for 1-4 hours until the column is fully conditioned.


Column Storage


Capillary columns should be stored in their original box when removed from the GC. Place a GC septa over the ends to prevent debris from entering the tubing. Upon reinstallation of the column, the column ends need to be trimmed by 2-4 cm to ensure that a small piece of septa is not lodged in the column.


If a column is left in a heated GC, there should always be carrier gas flow. The carrier gas flow can be turned off only if the oven, injector, detector and transfer lines are turned off (i.e., not heated).Without carrier gas flow, damage to the heated portion of the column occurs.


Table 8:


Solvent Volumes for Rinsing Columns


Column ID (mm)


0.18-0.2 0.25 0.32 0.45 0.53


Solvent Volume (mL)


3-4 4-5 6-7 7-8


10-12


Using larger volumes will not damage the column


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