Application of a catalytic oxidation method for the simultaneous determination of total organic carbon and total nitrogen in marine sediments and soils

Abstract

This study presents the application of a simultaneous method for the determination of total organic carbon (TOC) and total nitrogen (TN) in marine sediments and soils, using a data set of 206 samples collected from coastal lagoonal/marine sedimentary environments and certified reference materials (CRMs). TOC and TN were determined using the high temperature (720°C) catalytic (Pt/Al2O3) oxidation method and the detection of TOC and TN was performed using an infrared or a chemiluminescence detector, respectively. Results from the abovementioned TOC method were compared with the results from the widely used Wakley-Black titration method, while TN results with these from elemental analysis. Analytical quality control experiments were performed using CRM samples. Method characteristics such as range of measurement, calibration, method detection limit (MDL), limit of quantification (LOQ), repeatability and reproducibility, were calculated. The precision and the accuracy of the methods are also discussed. Comparison of the two TOC methods of 206 data set yields a regression line of correlation coefficient with R2 = 0.985. Additional different levels of TOC concentrations of low <1%, moderate 1–5% and high 5–40% level were examined indicating very good correlations. The lowest correlation coefficient was observed in low concentrations TOC<1% (R2 0.825), mainly as a result of the limitation of titration method. The evaluation of TN results indicated that the catalytic oxidation method and the elemental analysishave a significant good correlation with R2 = 0.977. The results of precision and accuracy, as well as the calculated MDL and LOQ show that this is a reliable method. Moreover, it requires a small amount of the analyzed sample and the total analysis time is 10 min. Therefore, it can be easily applied for the fast and precise simultaneous determination of TOC and TN in sediment and soil samples.