Direct and rapid determination of sulphate in environmental samples with diffuse reflectance Fourier transform infrared spectroscopy using KBr substrate

Abstract: The feasibility of employing diffuse reflectance Fourier transform infrared spectroscopy (DRS-FTIR) as a sensitive tool in the submicrogram level determination of sulphate (SO4 2−) was checked in this work. This paper presents the development of a new, rapid and precise analytical method for ppb levels of sulphate (SO4 2−) in environmental samples like coarse and fine aerosol particles, dry deposits and soil. The determination of submicrogram levels of sulphate is based on the selection of a quantitative analytical peak at 617cm−1 among the three observed vibrational peaks and preparing calibration curve using different known concentrations of sulphate by diffuse reflectance-Fourier transform infra red spectrometric (DRS-FTIR) technique. Pre-weighed and ground IR grade KBr was used as substrate over which remarkably wide range of known concentration of sulphate was sprayed and dried. The dried sample was analysed by DRS-FTIR. Three calibration curves for three different concentration ranges of sulphate were prepared for samples containing low and relatively higher sulphate contents. The relative standard deviation (n =8) for the sulphate concentration ranges, 2.5–35.5, 25.5–165, 55–1000μg/0.5g KBr, as used to prepare calibration curves, were 2.4%, 2.1% and 1.5%, respectively. The relative standard deviation for the sulphate concentration in real samples were found to be in the range, 3.11–5.76% (n =16), 4.05–7.75% (n =16) and 1.48–3.52% (n =10) for aerosol, dry deposits and soil, respectively. The LOD of the method is 0.20μg/g SO4 2−. The F- and t-tests were performed to check the analytical quality assurance test. The noteworthy feature of the reported method is the non-interference of any of the associated anions and cations. The results were compared with that of ion-chromatographic method with high degree of acceptability. The method can be applied in wide concentration ranges. A method for sulphate determination was introduced that did not require pretreatment of samples. This method employed the direct determination of the sulphate. The method is reagent less, nondestructive, very fast, repeatable, and accurate and has high sample throughput value. [Copyright &y& Elsevier]