K. Snavely et B. Subramaniam, ONLINE GAS-CHROMATOGRAPHIC ANALYSIS OF FISCHER-TROPSCH SYNTHESIS PRODUCTS FORMED IN A SUPERCRITICAL REACTION MEDIUM, Industrial & engineering chemistry research, 36(10), 1997, pp. 4413-4420
C-1-C-30 products from Fischer-Tropsch synthesis, conducted in a super
critical n-hexane medium over an Fe catalyst in a fixed-bed reactor, a
re analyzed using on-line gas chromatography. A Hewlett-Packard 5890 S
eries II gas chromatograph (GC) is modified to minimize the effects of
condensation of the on-line sample in the transfer lines. The GC is c
onfigured with a Supelco Petrocol DH capillary column connected to a f
lame ionization detector (FID) and two 1.83 m x 3.18 mm stainless stee
l columns placed in series, packed with. 80/100 mesh HayeSep D, connec
ted to a thermal conductivity detector(TCD). It is shown that pressure
and temperature affect the elution order of oxygenates relative to hy
drocarbons in the nonpolar capillary column. This phenomenon is exploi
ted for obtaining improved resolution; several distinct methods produc
e similar elution orders. Ar, added to the syngas feed, is used to cal
culate syngas conversion. All compounds eluting before hexane (C-1-C-5
, Other than 2-methylpropene/1-butene and propanal/propanone) and near
ly all the major peaks eluting after hexane are resolved in the capill
ary column. H-2, Ar, CO, CH4, CO2, and H2O are resolved in the packed
columns. The method provides excellent quantitative measurement of com
ponent mole fractions that are within the range of calibration.