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The growth of carbon nanotubes (CNTs) by direct liquid injection chemical vapor deposition (DLICVD) has been studied using the polyoxometalate cluster [HxPMo12O40⊂H4Mo72Fe30(O2CMe)15O254(H2O)98-y(EtOH)y] (FeMoC) as the catalyst with either ethanol or toluene as the carbon source. In order to screen different growth conditions a single large batch of FeMoC is required in order to eliminate variation in the catalyst precursor. The preparation of 6 g of FeMoC is possible by scaling (10×) literature reagent ratios. DLICVD studies of the FeMoC derived carbon product were evaluated by Raman spectroscopy and scanning electron microscopy (SEM) to determine the quality (G:D ratio) and purity of CNT content. With the use of ethanol as the carbon source, increasing the temperature in the injection zone (aspiration temperature) above 250 °C increases the yield, and results in a slight increase in the G:D ratio. The maximum yield is obtained with a growth temperature of 900 °C, while the G:D ratio is the highest at higher temperatures. Faster solution injection rates increase yield, but with a significant decrease in G:D, in fact no CNTs are observed in the product for the highest injection rate (10 mL/h). An optimum catalyst concentration of 1.25 wt.% is found, which influences both the catalyst:C and catalyst:H ratios within the system. Growth at 800 °C is far more efficient for toluene as a carbon source than ethanol. The resulting “process map” allows for large quantities of CNTs to be prepared by DLICVD.