How does grinding affect the mid-infrared spectra of soil and their multivariate calibrations to texture and organic carbon?

Abstract

Mid-infrared (mid-IR) diffuse reflectance spectroscopy can be used to effectively analyse soil, but the preparation of soil samples by grinding is time consuming. Soil samples are usually finely ground to a particle size of less than 0.250 mm because the spectrometer’s beam aperture is approximately 1–2 mm in diameter. Larger particles can generate specular reflections and spectra that do not adequately represent the soil sample. Grinding soil to small particle sizes enables the diffuse reflectance of light and more representative sample measurements. Here, we report on research that investigates the effect that grinding to different particle sizes have on soil mid-IR spectra. Our aims were to compare the effect of grinding soil to different particle sizes (2.000 mm, 1.000 mm, 0.500 mm, 0.250 mm and 0.106 mm) on the frequencies of mid-IR spectra, and compare the effect of these particle sizes on the accuracy of spectroscopic calibrations to predict organic carbon, sand, silt and clay contents. Using the Commonwealth Scientific and Industrial Research Organisation’s (CSIRO) National visible–near infrared database, we selected 227 soil samples from the National Soil Archive for our experiments, and designed an experiment whereby each soil sample was ground in triplicate to the different particle sizes. These ground samples were measured using an FT-IR spectrometer with a spectral range of 4000–600 cm–1. Grinding to particle sizes that are ≤2.000 mm reduces subsample variability. Smaller particle sizes produce finer and sharper absorption features, which are related to organic carbon, and clay and sand mineralogies. Generally, better predictions for clay, sand and soil organic carbon contents were achieved using soil that is more finely ground, but there were no statistically significant differences between predictions that use soil ground to 1 mm, 0.5 mm, 0.25 mm. Grinding did not affect predictions of silt content. Recommendations on how much grinding is required for mid-IR analysis should also consider the time, cost and effort needed to prepare the soil samples as well as the purpose of the analysis.