Rapid and portable mid-infrared analysis of wet sediment samples by a novel “filter-press” attenuated total reflectance method

Abstract

Mid-infrared (MIR) analysis of wet sediments or soils usually requires freezing and drying, adding considerable analysis time and cost, and promoting changes in chemical properties. A novel attenuated total reflectance (ATR) mid-infrared (MIR) method was developed to enable analysis of non-processed, aqueous sediments. Wet sediment samples from the Coorong Lagoon, South Australia, were subjected to laboratory analysis for physical and chemical properties, our new filter-press ATR method, and conventional ATR and diffuse reflectance (DRIFT) analysis of dried samples. For ATR on wet sediments, samples were pressed onto the ATR crystal with a filter-paper backing and scanned. The spectra were analyzed by principal components analysis (PCA) and partial least squares regression (PLSR) to develop multivariate models for total organic carbon (TOC). ATR spectra of as-received wet sediments were poor due to water absorption features, but filter-pressing reduced these and greatly enhanced the solids spectral component. The filter-pressed PLSR cross-validation for TOC resulted in an R2 = 0.89 and RMSECV = 0.78%. Prediction accuracies were similar to freeze-dried ATR samples and far more accurate than testing wet samples without filter-pressing. Our findings confirmed the filter-press ATR method as proof-of-concept and showed that it has the potential to remove one of the major barriers to in-field application of MIR techniques, the high and variable amounts of moisture levels commonly present in many environmental samples. Extension of the filter-press ATR method to a wider range of analytes may enable it to rapidly acquire moist or wet sediment and soil property data while in the field.