A method was developed for the analysis of mutagenic nitroarenes in carbon black. The procedure included extraction, pre-separation column chromatography on silica gel, and determination by high-performance liquid chromatography (HPLC) using a diode-array detector. Different solvents, such as dichloromethane, benzene, toluene, and chlorobenzene were used for the extraction of carbon black. It was found that chlorobenzene yielded the highest amount of extracted material. The pre-separation, the optimization of the HPLC separation, the selection of detection wavelengths, and the calibration curve are discussed. 3-Nitro-9-fluorenone was detected in a treated carbon black, which is used for making carbon ink. The identification of peaks in the sample chromatograms was confirmed by comparing the retention time and the UV spectra with those of standards.