Abstract Although infrared spectrophotometry is suitable for the measurement and identification of pesticides and their metabolic products because of its inherent characterizing properties, only recently have techniques and instrumentation become adequate for the difficult requirements of residue chemistry. This paper describes techniques which have been successful for the quantitative measurement and qualitative characterization of micro-quantities of pesticide residues. Because of the nature of residue problems, microtechniques are essential for the successful use of infrared spectrophotometry; these techniques strictly limit the permissible amount of contamination from substrate, reagent, atmosphere, handling, etc. Such techniques are described as well as amounts of material required for reliable infrared data. Quantitative measurements are most reliably made as solutions in long energypath cells, whereas qualitative characterization is best accomplished as micro pellets. Detailed procedures for each of these techniques are described.