Nondestructive and rapid determination of nitrate in soil, dry deposits and aerosol samples using KBr-matrix with diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS)

This paper presents the development of a new, rapid and precise analytical method for submicrogram levels of nitrate (NO3-) in environmental samples like soil, dry deposit samples, and coarse and fine aerosol particles. The determination of submicrogram levels of nitrate is based on the selection of a quantitative analytical peak at 1385 cm(-1) among the three observed vibrational peaks and preparing calibration curves using different known concentrations of nitrate by diffuse reflectance Fourier transform infra red spectrometric (DRIFTS) technique. Pre-weighed and ground infrared (IR) grade KBr was used as substrate over which remarkably wide range of known concentration of nitrate was sprayed and dried. The dried sample was analyzed by DRIFTS and absorbance was measured. Eight calibration curves for four different concentration ranges of nitrate for absorbance as well as peak area were prepared for samples containing lower and relatively higher values of nitrate. The relative standard deviation (n = 8) for the nitrate concentration ranges, 0.05-40, 0.05-1.5, 1.5-25, 5-40 mu g/0.1 g KBr were in the range 1.6-2.3% for the above calibration curves. The limit of detection (LOD) of the method is 0.07 mu g g(-1) NO3-. The F- and t-tests were performed to check the analytical quality assurance test. The noteworthy feature of the reported method is the noninterference of any of the associated 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. The method is reagent less, nondestructive, very fast, repeatable, and accurate and has high sample throughput value. (c) 2006 Elsevier B.V. All rights reserved.