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Lignin-derived and standard phenols were successfully analyzed with reversed-phase high-performance liquid chromatography (HPLC) with diode array detection. The 11 major phenols produced by cupric oxide (CuO) oxidation were clearly and rapidly separated. Determination by diode array detection also allowed detection of interfering impurities within individual HPLC peaks. The lignin phenols were accordingly corrected and quantified. This method yields precise and reliable data for various environmental samples such as dissolved organic matter from aqueous samples and sediments and can also be applied to various particulate materials such as detritus and plant tissues. An interlaboratory method comparison with humic substance standards from the International Humic Substances Society revealed differences in lignin phenol concentrations, whereas lignin parameters better coincided.