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Inorganic carbonate can be an important component of atmospheric particulate matter in arid environments where mineral dust components contribute significantly to air particulate matter. Carbonate carbon (CC) is only rarely quantified in atmospheric studies and methods to quantify carbonate in atmospheric samples are rare. In this manuscript, we present a novel protocol for quantifying carbonate carbon in atmospheric particulate matter samples, through the acidification of aerosol filters at ambient pressure and temperature and subsequent measurement of carbon dioxide (CO2) released upon acidification. This method is applicable to a variety of filter media used in air pollution studies, such as Teflon, cellulose, or glass fiber filters. The method allows the customization of the filter area used for analysis (up to 24 cm2) so that sufficient CO2 can be detected when released and to assure that the sample aliquot is representative of the whole filter. The resulting detection limits can be as low as 0.12 µg/cm2. The analysis of a known amount of sodium bicarbonate applied to a filter resulted in a relative error within 15% of the known mass of bicarbonate when measured 20 min after acidification. A particulate matter sample with aerodynamic diameter larger than 2.5 µm (PM>2.5) collected via cascade impaction on a high-volume aerosol sampler yielded good precision, with a CC concentration of 4.4 ± 0.3 µgC/cm2 for six replicates. The precision, accuracy, and reproducibility of this method of CC measurement make it a good alternative to existing quantification methods.