Figures

Figure 1

Stainless steel gas handling manifold attached to the injection head of a Hewlett Packard 5890 Series II Plus GCMS. All zones (sampling valve, injection head, capillary column, and source inlet) were maintained at 75 °C.

Figure 2

Chromatograms of MgCp2 in bubblers from Company "A". Different processes were used to synthesize the MgCp2 in each bubbler. The MgCp2 in bubbler A2 was produced without using diethyl ether (CH₃CH₂OCH₂CH₃). Impurities in each bubbler could be removed by evacuating for a short period of time (~15 min.) at elevated temperatures (~50 °C) as shown in figure 3.

Figure 3

A chromatogram of pure MgCp2 obtained after evacuating bubbler A1 in figure 2. Identical chromatograms were obtained after evacuating bubbler A2 as well as from the optimized MgCp2 processes of companies B and C (bubblers B3 and C2 described in figures 4 and 5).

Figure 4

Chromatograms of MgCp2 in bubblers from Company "B". Different processes were used to synthesize the MgCp2 in each of the three bubblers. Neither of the processes for bubblers B2 and B3 used diethyl ether. However, only B3 could be purified fully by evacuation. The final result is identical to the chromatogram shown in figure 3.

Figure 5

Chromatograms of MgCp2 in bubblers from Company "C". Different processes were used to produce the MgCp2 in bubblers C1 and C2. No hydrocarbon impurities were detected in C2.

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