Temperature programming for high-speed GC

Citation
C. Leonard et al., Temperature programming for high-speed GC, ANALYT CHEM, 71(11), 1999, pp. 2123-2129
Citations number
36
Categorie Soggetti
Chemistry & Analysis","Spectroscopy /Instrumentation/Analytical Sciences
Journal title
ANALYTICAL CHEMISTRY
ISSN journal
00032700 → ACNP
Volume
71
Issue
11
Year of publication
1999
Pages
2123 - 2129
Database
ISI
SICI code
0003-2700(19990601)71:11<2123:TPFHG>2.0.ZU;2-Q
Abstract
Fast temperature programming (20-50 degrees C/min) is used with relatively short separation columns to achieve highspeed separations of mixtures cover ing a nide boiling point range. A cryofocusing inlet is used to obtain narr ow injection plugs. High-speed temperature-programmed chromatograms are eva luated by considering local peak capacity as a function of carbon number an d boiling point I for the normal alkanes in the range C-8-C-19. The peak-ca pacity generation rate (peaks per second) as a function of carbon number an d the total cumulative peak capacity as a function of time are also conside red for various column lengths and carrier gas now rates. Column lengths in the range 3.6-25.4 m and average carrier gas velocity values in the range 50-200 cm/s are considered. For a 6.8-m-long, 0.25-mm-i.d. column operated at an average i carrier gas velocity of about 100 cm/s and using a: nominal programming rate of 50 degrees C/min, C-19 elutes in: 178 s with a total p eak capacity of 168 peaks. If the programming rate is reduced to 20 degrees C/min, the C-19 elution time more than doubles but the total peak capacity increases by only 20%. For a 25.4-m-long column using a nominal 50 degrees C/min programming rate, the C-19 retention : time is 262 s with a peak cap acity of 279 peaks. The use of average carrier gas now rates greater than a bout 100 cm/s, which is common in isothermal high-speed GC, results in a co nsiderable loss in total peak capacity with remarkably little reduction in analysis time.