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samples are taken at at known times and the concentration is calculated via UV-Visible spectroscopy. Equilibrium is reached when the concentration pleataus. For byproduct dependence reactions, the byproduct is loaded into an HPLC sample loop and then a known volume of byproduct is injected into the reactor. Next, hydrogen is loaded into the system using a manifold of known volume (70 mL). The moles of hydrogen injected are then calculated by pressure drop using the ideal gas law. The aluminum stage is then quickly heated (~ 15 s.) to the desired reaction temperature and maintained for 3 minutes. The heated stage is then allowed to cool down (~ 15 s.) while fresh CO2 is used to flush multiple reactor volumes through the system to remove reaction byproducts and unreacted precursor. The effluent is passed through an activated carbon bed and silicon oil bubbler before being vented to the atmosphere. During the reaction, small gas phase samples of known volume are collected using HPLC sample loops. Samples were decompressed and the precursor is recovered in a known volume of n-heptane and the resulting solutions are analyzed using UV visible spectroscopy (257 nm and 305 nm, Figure 2.5) in order to determine precursor concentrations (Figure 2.6 shows the standard curve for Ru(tmhd)2cod in n-heptane where the extinction coefficients for the Beer-Lambert law are 18.71 L/g for the primary absorbance of 257 nm and 9.69 L/g for the secondary absorbance of 305 nm) in the fluid phase and confirm conversions of less than 15 %. A differential method of rate analysis is used to analyze the data and propose a reaction mechanism as well as determine the reaction rate orders for the growth rate. The method of excess is used to account for multiple reactants. 25PDF Image | Supercritical Fluid Deposition Of Thin Metal Films
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