An Evaluation of the Loss-on-Ignition Method for Determining the Soil Organic Matter Content of Calcareous Soils

The Loss-on-Ignition (LOI) method is widely employed for measuring the organic matter (OM) content of soil samples. There is a risk of carbonate losses when calcareous soil samples are analyzed through LOI, but this has never been investigated in detail. Moreover, a worldwide standard protocol for determining the carbonate content of soils is not available. The aims of this study were (i) to evaluate two commonly employed carbonate analysis procedures using calcareous and non-calcareous soil samples: the gravimetric method with (GMF) and without (GM) the addition of the antioxidant iron(II) chloride (FeCl₂) and the acetic acid dissolution procedure (AAD); (ii) to evaluate the effect of ignition temperature on losses of pure calcite, calcite-quartz and calcareous soil samples. We found that the average apparent carbonate content of the non-calcareous soils was greatest for the GMF method followed by the AAD procedure. The GM method showed the smallest apparent carbonate contents. For the calcite-quartz sand mixture, ignition losses started at 600°C and increased with temperature in a sigmoidal way. LOI values stabilized at 750°C when 80% of the carbon dioxide was released. We recommend the GM procedure for carbonate analysis because the apparent carbonate contents of the non-calcareous soil samples were smallest. Furthermore, we recommend an LOI temperature of 550°C because at this ignition temperature 99.8% of the total calcite fraction remains in the soil samples.