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Recently discovered phosphate-derived Ni catalysts have opened a new pathway towards multicarbon products via CO2 electroreduction. However, understanding the influence of basic parameters such as electrode potential, pH, and buffer capacity is needed for optimized C3+ product formation. To this end, rigorous catalyst evaluation and sensitive analytical tools are required to identify potential new products and minimize increasing quantification errors linked to long-chain carbon compounds. Herein, we contribute to enhance testing accuracy by presenting sensitive 1H NMR spectroscopy protocols for liquid product assessment featuring optimized water suppression and reduced experiment time. When combined with an automated NMR data processing routine, samples containing up to 12 products can be quantified within 15 min with low quantification limits equivalent to Faradaic efficiencies of 0.1%. These developments disclosed performance trends in carbon product formation and the detection of four hitherto unreported compounds: acetate, ethylene glycol, hydroxyacetone, and i-propanol. Phosphate-derived nickel catalysts enable access to multicarbon products via CO2 electroreduction, but it remains unclear how operating conditions influence product formation. Here, refined 1H NMR spectroscopy protocols are introduced and combined with an automated NMR data processing routine, enabling quantification of carbon product formation as a function of various parameters. [ABSTRACT FROM AUTHOR]