Health & Environmental Research Online (HERO)


Print Feedback Export to File
4216947 
Journal Article 
Investigation of high-speed gas chromatography using synchronized dual-valve injection and resistively heated temperature programming 
Reid, VR; Mcbrady, AD; Synovec, RE 
2007 
Yes 
Journal of Chromatography A
ISSN: 0021-9673
EISSN: 1873-3778 
1148 
2 
236-243 
English 
17386929 
WOS:000246242700014 
High-speed temperature programming is implemented via the direct resistive heating of the separation column (2.3m MXT-5 Silicosteel column with a 180 microm I.D. and a 0.4 microm 5% phenyl/95% dimethyl polysiloxane film). Resistive temperature programming was coupled with synchronized dual-valve injection (with an injection pulse width of 2 ms), producing a complete high-speed gas chromatography (GC) system. A comparison of isothermal and temperature programmed separations of seven n-alkanes (C(6) and C(8)-C(13)) shows a substantial improvement of peak width and peak capacity with temperature programming. The system was further implemented in separations of a mixture of analytes from various chemical classes. Separations of the n-alkane mixture using three different temperature programming rates are reported. A temperature programming rate as high as 240 degrees C/s is demonstrated. The method for determination of temperature programming rate, based on isothermal data, is discussed. The high-speed resistive column heating temperature programming resulted in highly reproducible separations. The highest rate of temperature programming (240 degrees C/s) resulted in retention time and peak width RSD, on average, of 0.5 and 1.4%, respectively, for the n-alkane mixture. This high level of precision was achieved with peak widths-at-half-height ranging from 13 to 36 ms, and retention times ranging from 147 to 444 ms (for n-hexane to n-tridecane). 
Band broadening; Gas chromatography; High speed; Resistive heating; Retention time precision; Temperature program