Optimizing the weight loss-on-ignition methodology to quantify organic and carbonate carbon of sediments from diverse...

The sequential weight loss-on-ignition (WLOI) method for determination of organic and carbonate or inorganic carbon (C) content was evaluated on sediments from diverse sources with a great range of C contents. The sediments were collected from canal, wetland, river, estuary, lake, and marine sites. The organic and inorganic C contents of these samples ranged from 1 to 430 g kg( -1) and from 4 to 97 g kg( -1), respectively. Combinations of the combustion time and temperature and optimal weight ranges of representative samples were tested, and comparisons of the WLOI method with other methods, including dry combustion and wet combustion, were made. These methods were (1) use of the carbon-nitrogen-sulfur (CNS) autoanalyzer with normal and reduced temperatures for total and organic C, (2) thermogravimetry for both organic and inorganic C, (3) use of the CNS autoanalyzer after removal of inorganic (carbonate) C by fumigating samples with concentrated HCl for organic C, (4) Walkley-Black wet combustion method for organic C, and (5) pressure-calcimeter associated with subtraction method (total C minus inorganic C) for organic C determinations. The results of analyzing samples of sediments of diverse origins showed that the optimal combination of temperature and time of WLOI depended mostly on the sources of the analyzed sediment. The WLOI analysis of sediment samples for organic C from wetlands, canal, estuary, or river sites needed a relatively low temperature but that of sediment samples from lake and marine sites required a relatively high temperature. Overall, to obtain reliable analysis results of samples from widely varied sediment sources except marine sediments, 500°C for 12 h was optimal for organic C content determination, and 800°C for yet another 12 h was optimal for inorganic C content determination. The temperature could even be reduced to 475°C if only wetland and stream sediments were included, but for marine sediments, 550°C for 12 h was necessary. Precise C content determinations for most sediment sources could be obtained by WLOI when sample quantities ranged from 2.0 to 4.0 g. The WLOI method, when conducted properly, resulted in precise measurements of C contents in "standard samples" used for calibration, and these values were closely comparable to results obtained with other dry combustion methods (R (2) ≥ 0.96). We conclude that WLOI, which has advantages of simplicity, cost-effectiveness, and no waste disposal over other methods, can provide precise measurements of organic and inorganic C contents in sediments from a wide range of sources, but the selection of heating temperature and exposure time should be carefully considered based on sediment sources.