Many analytic applications benefit from the ability to measure very small samples non-destructively. Typical applications of near-infrared analysis require sample sizes of 5 to 50 grams. The purpose of this evaluation was to determine if sub-gram quantities of sample could be used with the ASD LabSpec 4 Standard-Res i. A set of dried ground corn stover samples was used for this study to evaluate this small sample size capability. ASD’s spectrometer system was used with very small samples in micro-centrifuge tubes to allow higher throughput in the lab thus reducing costs associated with the NIR analysis.