Evaluation of sample pre-treatment and potential contamination of soluble carbon in soil extracts during lyophilisation

Lyophilisation of K₂SO₄ soil extracts has been proposed as a sample preparation technique before elemental analysis of carbon or nitrogen. However, previous measurements, based on wet oxidation or catalytic combustion, indicated that C measurements in lyophilised samples not always proved to be accurate. To determine whether the C analysis was affected by the lyophilisation process, an exploratory study was conducted to investigate the potential effects of the sample pre-treatment and of the lyophilisation process itself. This paper puts forward that the use of soil extracts, previously stored at −20 °C, may affect the recovery of salt in the samples and that contamination of the soluble carbon with exogenous C during lyophilisation is feasible. Therefore we recommend to use freshly prepared soil extracts for lyophilisation and always to include an internal standard among the unknown samples to account for a possible contamination.