An automated large volume on-column injection technique for capillary gas chromatography

Automated large volume (25-200 μl) on-column injections into a gas chromatograph with a capillary column were successfully performed by coupling a retention gap technique with an air actuated rotary valve. The linearity, injection precision, and carryover were evaluated. Slight boiling point discrimination was observed. This technique is compatible with commonly used chromatographic detectors (FID, ECD, MS) and conditions, while requiring very little instrument modification. The work is directed at the eventual reduction of manpower and turnaround time for sample collection and extraction, and Kuderna-Danish concentration when dealing with methods similar to EPA 625.     

Gas chromatographic separation of sugars by on-column injection on glass capillary columns

Sugars were separated gas chromatographically on short apolar glass capillary columns by using cold, on-column injection (OCI) techniques. After silylation, oligomers up to the hexasaccharides could be efficiently separated in resonable retention times. Response factors of silylated sugars were determined as a function of varying sample amounts and concentrations. The optimum injection amount was found to be 1 μl in heptane as solvent.     

Linearity of a flame ionisation detector for capillary gas chromatography

Summary The influence of the nitrogen and hydrogen flow rates on the linearity of the flame ionisation detector is investigated and flow-rates which give a linear response over five orders of magnitude are determined.     

Studies on cryogenic trapping of solutes during chromatographic elution in capillary gas chromatography

Cryogenic trapping of solutes leads to narrowing of the chromatographic band. By placing the trap at the end of a capillary column, it is possible to study the effectiveness of the trap in terms of producing a sharpened elution profile. The trap may be heated by supplementary heating, but here convective heating from the GC oven is employed simply by turning off the cryogenic coolant. It is estimated that it takes about 50 s for the trap to heat up sufficiently to allow trapped solute to be remobilized, although this depends upon the oven temperature and thermal mass of the trap. It can also be shown that the more volatile solutes mobilize faster from the trap in this particular mode of operation. The recovery of trapped components shows that there is essentially quantitative trapping, and the solutes are trapped just at the leading edge of the trap.     

Direct injection on capillary columns for gas chromatography

Discrimination may occur when injecting samples onto gas chromatography capillary columns, whereby peak areas for higher boiling point compounds are smaller than they should be compared to lower boiling compounds. This problem is most important in quantitative work on solutes having a wide range of volatility. An all-glass inlet system was used. Injections were made with a 10-μl syringe onto a column without and injection point heater and with the column oven about 20°C below the boiling point of the solvent used for the solutes. Discrimination did not occur in a range of C₁₂ to C₃₆ n-alkanes.     

Analysis of antiepileptic drugs by capillary gas chromatography with on-column injection

A simple and quick gas chromatographic method has been developed for the determination of up to six commonly used antiepileptic drugs in human serum. The antiepileptics are isolated from serum by solid phase extraction on to a reversed phase sorbent and recovered with ethyl acetate as eluent. The ethyl acetate eluate is suitable for direct on-column injection on to a phenyl methyl siloxane capillary column; hydrogen is used as carrier gas and the compounds are separated with a two-ramp temperature program. Detection is by FID. The reproducibility of the method varies between 2 and 6% RSD, depending on the drug and the level analyzed; limits of detection were found to be 14–51 pg and minimum assayed concentrations in serum were between 14 and 51 ng/ml.     

The solvent venting injection technique in capillary supercritical fluid chromatography

A solvent venting technique for injection of volumes up to 1 μl on 50 μm i.d. SFC columns has been compared to direct injection methods. The peak broadening and peak splitting observed with direct injection have been examined and found to be related to the starting pressure, the column temperature, and the sample solvent, in addition to the sample volume. The solvent venting technique removed peak splitting and improved the column efficiency. With a proper selection of experimental conditions, the sample recovery was 100%. The major part of the solvent was eluted in 15–20 s. Several applications have been demonstrated.