An advanced solventless column test for capillary GC columns.
Manufacturing skills for capillary GC columns have improved to a point where the commonly used tests no longer distinguish between "adequate" and "excellent" columns. A more stringent test mixture, coupled with a more exacting procedure, was proposed for testing capillary columns in 2004. The solutes were less sterically hindered and less retained, permitting the test to be run isothermally at lower temperatures where sorptive forces are stronger. To avoid masking active sites by solvent flooding, the test used a higher boiling solvent that eluted last. This test mixture, used under the prescribed conditions, differentiated adequate from excellent columns, but removal of the late-eluting solvent prolonged run times to as long as 1 h. The new test uses the same probes proposed in 2004, but entirely eliminates the solvent. Injections utilize a plunger-in-needle microvolume syringe, and the "gas saver" feature of a contemporary gas chromatograph. The latter serves as a dynamic diluter to deliver nanogram quantities of undiluted solutes to the column. The test can be conducted isothermally at a lower temperature in less than 15 min for most of the columns. This paper summarizes the analytical approach used, and presents method performance data and test results obtained on contemporary capillary columns from leading manufacturers.
Luong
Jim
J
Dow Chemical Canada, Fort Saskatchewan, Alberta, Canada.
Gras
Ronda
R
Jennings
Walter
W