Practical aspects of splitless injection of semivolatile compounds in fast gas chromatography

J Chromatogr A. 2004 Nov 5;1055(1-2):159-68. doi: 10.1016/j.chroma.2004.07.058.

Abstract

Possibilities and practical aspects of implementation of splitless injection of larger volumes for fast GC purposes utilizing narrow-bore column, hydrogen as carrier gas, fast temperature programming under programmed flow conditions and commercial instrumentation were searched. As a model sample semivolatile compounds of a broad range of volatility and polarity (7 n-alkanes and 19 pesticides) were chosen. Peak shapes, peak broadening and peak areas and its repeatability were evaluated under various experimental set-ups (liner/injection technique combinations). Various factors, such as liner design, injection technique, retention gap length, compound volatility and polarity, the solvent used, initial oven temperature influenced compound focusation and/or maximal injection volume. Combination of analytical column (CP-Sil 13 CB 25 m long, 0.15 mm i.d., film thickness 0.4 microm) with normal-bore retention gap (1 m long, 0.32 mm i.d.) allowed maximal injection volume 8 microl for 4 mm i.d. liner used without any peak distortion when solvent recondensation in the retention gap was employed.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Chromatography, Gas / methods*
  • Solvents
  • Temperature
  • Volatilization

Substances

  • Solvents