AbstractTwo methods are proposed for assessing the total concentration (cAr) of the most toxic hydrocarbons (arenes) in wastewaters. The procedures include the extraction of petroleum products with n-hexane, the adsorption purification of the extract from phenols, and the measurement of the absorbance of arenes in the UV region. No separation of alkanes and cycloalkanes is required. The first method enables the rapid estimation of cAr in terms of the standard substance Xst (o-xylene or m-xylene) for screening purposes. Absorbance is measured at 250 nm, which decreases the effect of intragroup selectivity and phenols remaining in the extract. The total concentrations of arenes in n-hexane solutions are estimated by this method rather accurately (error δc < 7% at RSD < 5%). However, the analysis of aqueous solutions (wastewater simulant solutions) in the range of cAr from 0.1 to 50 mg/L leads to δc > 50%. The results of cAr estimation in simulations and wastewaters are underestimated, which is mainly due to the loss of arenes during sample preparation. Using the second (more accurate) method, the absorbance of the extract is measured at seven wavelengths in the region 240–280 nm. The cAr value is found by multiple linear regression without recalculation to Xst. Multivariate calibrations are constructed using extracts from 25 simulated solutions (training set) and passing them through all sample preparation operations, which decreases the loss of analytes. At cAr > 1 mg/L, the error in the analysis of simulants from the test set does not exceed 20% at RSD < 12%. The duration of analysis is 1 h. The procedure was tested in the analysis of wastewaters from enterprises of various profiles. The results agree with the results of chromatographic analyses of the same samples.