Oil contamination of sediments by freeze-drying versus air-drying for organic geochemical analysis

Freeze-drying is widely used in geochemical laboratories for preparing wet solid environmental samples such as sediments and soils before being analyzed for their contents and states of various metal elements and labile organic components that may be temperature- and/or redox-sensitive. Screening bulk geochemical analysis of two Artic lake sediment samples prepared by freeze-drying displayed unexpectedly high contents of labile organic matter (OM) represented by the Rock-Eval S1 peaks (e.g., 8.12 and 4.84 mg HC/g sediment). The amount of labile OM was reduced greatly for the freeze-dried sediment samples after a thorough cleaning of the freeze-drier sample chamber (e.g., 2.75 and 1.46 mg HC/g sediment), but was still significantly higher than that of the equivalent air-dried samples (e.g., 0.76 and 0.23 mg HC/g sediment). Compositional analysis of the labile OM fractions by gas chromatography (GC) of both freeze-dried and air-dried aliquots of the same sediments indicates the presence of unresolved complex mixture (UCM) humps of C₁₀-C₂₃ hydrocarbons in the freeze-dried samples. In contrast, air-dried samples, either real sediments or blank laboratory materials represented by clean sand and thermally spent shale, do not show the C₁₀-C₂₃ hydrocarbon UCM humps on their GC traces. The hydrocarbon UCM humps persist in the freeze-dried samples even they further went through air-drying at ambient conditions. Both bulk and compositional analytical results in this work appear to indicate the potential risk of introduction of external hydrocarbons to the prepared materials during freeze-drying process, especially if an aged freeze-drier was used without being thoroughly cleaned and if pump oil and cooling fluids were components of the device.