Rapid Separations on a Portable GC with Resistively Heated Columns

J. N. Driscoll PID Analyzers, LLC & Stanley Stearns Valco Instruments, Inc.

Introduction
Much of the previous work on fast GC utilized short (5M) thin film capillary columns to elute solutes quickly and the result is rapid but inferior separations because of the short column. New technology developed at Valcos capillary column development center where VICI takes polyimidecoated fused silica (FST) and removes the polyimide layer. Then the (FST) is electroplated with nickel. As a result of the superior heat transfer of the electroplated nickel, we are able to rapidly and efficiently heat and achieve excellent resolution for a 30M capillary column. These columns can be programmed faster (hundreds of degrees/min)- save 50-90% The columns can be reliable started a few degrees above ambient These columns cool down faster because of their low mass so savings> 50% Stearns et al (J. Chromat.) have looked at high MW HC but we are looking at applications for low MW HC with thick films (5-10m)

Photo of Resistively Heated GC Gas Analysis System

Photo GC 312

Fast GC Electronic Schematic

PW Software for GC Cont. & Integration

VICI Column SW w PW Display
PeakWorks Chromatography SW

Fast GC for High MW HC

Comparison of Applications
The previous slide from Stearns shows the dramatic effect of TP for high MW organics up to C30 where analysis times can be reduced by 5090% and cool down times by >50%. Our applications at PID are in lower MW HC up to C6 but also C1. Here we have to start just above to ambient, a difficult task for most GCs, w/o subamb. We were able to start @ 23oC (reproducibly), hold 1 min, then prog. to 200oC (<1 min.) & hold for 2min. to complete. Results shown in the following slide

Isothermal Chromatogram C1 to C6 on GC312

C1 to C6 HC by cap GC

Fast GC Chromatogram for C1 to C6 alkanes

Temp. Programming Comparison

Chromatogram of Gasoline Vapor

12000

FID- Gasoline Vapor from Tank HS

10000

8000 FID Response

6000 Series1 4000

2000

0 0 50 100 150 200 Time -sec 250 300 350 400

Solvents (BTX + MeOH)

Conclusions
We have shown similar results with low MW HCnamely 50% reduction in analysis times There are eight different ramps that can be programmed so that separations can be improved in different sections Although we have worked with thick films, these columns are available with thin films for high MW compounds and with PLOT columns for separation of low MW gases Very fast < 10 second chromatograms can also be produced easily for studying reaction kinetics in chemical analyses.