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Paraho Shale Oil Analysis

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The analysis of Paraho shale oil naphtha 260°C (500°F) was performed using a 60-m DB1 fused silica capillary column from and W Scientific in a 5700A Hewlett Packard gas chromatograph. The column was coupled directly to the source of a VG 7070H double-focusing mass spectrometer tuned to a resolution of 1000.
The column was programmed from 30 to 200°C at 1°Cmin. The sample was splitless injected with the injection port at 300°C. Helium was used as the carrier gas at a pressure of 1.4 kg/cm. Optimum resolution was attained at an approximate linear flow velocity of 20 cms. Data were collected using a magnet scan cycle of 1.5s from mass 12 to 300 using an INCOS instrument control and data collection computer system. The multiple ion detection (MID) data were acquired at a mass spectrometric (MS) resolution MAM = 9600 at a repetition rate of 1.5 s. …show more content…
The injection port is designed so that the needle is received by a .76-mm (0.03-in.) sleeve which couples to the fused silica capillary column. Figure 1 shows a schematic diagram of the injection port designed to accept both the .25-mm (0.010-in.) outside diameter (OD) fused silica columns and a .76-mm (0.03-in.) OD stainless steel columns.
Sample
The Paraho shale oil naphtha 260°C (500°F) distillate sample was obtained from the Laramie Energy Research Center specifically for method development and use by ASTM Committee E-14 on Mass Spectrometry.

Figure 2 shows the flameionization detector (FID) gas chromatogram of the Paraho shale oil naphtha using a 60-m DB1 fused silica capillary column. This is compared to that obtained using a second 60-m DB1 column on the gas chromatographicmass spectrometric (GCMS) system. Note comparable resolution of the traces. Figure 3 is a closeup of the peaks circled in Fig. 2. There is some shifting of peak positions; but, by and large, the resolution is the