The goal of this research study was to evaluate air and soil sampling methods and analytical techniques for commercial land application of biosolids. Biosolids were surface applied at agronomic rates to an agricultural field. During the period of August 2004 to January 2005, 35 groups of analytes were measured using 13 sampling techniques. Several analytes were measured in more than one matrix. For example, fecal coliforms were measured in biosolids, air, and soil. In total, 49 analyte-matrix combinations were measured. The multimedia approach and numerous analyte-matrix combinations are unique for a field study on the land application of biosolids. For 27 combinations, data met quality criteria, and interpretation used conventional methods. Quality assurance (QA) criteria were not met, or QA data were not reported for 12 combinations. The interpretation of these data sets was affected by QA limitations, and conclusions from these data are more uncertain. No detections were observed for 10 microbial analytes. It is not clear if organisms were present but not detected or were absent. In this study, odors were detected in the air, and chemicals and microbes were measured in the soil after land application of biosolids. Odors had dissipated after 4 days. In shallow soils, most microbial and chemical analytes remained elevated for the remainder of the study, 98 days. The conclusions of this study may have been affected by the biosolids applied, weather conditions during and after application, and other site-specific variables. Additional studies would be useful to determine if these observations are consistent with other biosolids applications. Based on the results of this study, the 27 analyte-matrix combinations yielding usable data have been demonstrated at field scale and could be used in future research within the QA context of this study. For the other analyte-matrix combinations, additional QA samples, screening of analytical labs for compliance with QA, and continued methods development are needed. This research, in combination with the work of others, may result in the development of an integrated, multimedia protocol for use in field sampling of biosolids land application.