The Rio Grande Valley study unit of the U.S. Geological Survey National Water-Quality Assessment Program conducted a two-phase synoptic study of the occurrence and distribution of pesticides and nutrients in the surface water of the Mesilla Valley, New Mexico and Texas. Phase one, conducted in April-May 1994 during the high-flow irrigation season, consisted of a 6-week time- series sampling event during which 17 water-column samples were collected at 3 main-stem sites on the Rio Grande and a synoptic irrigation-run sampling event during which 19 water-column samples were collected at 7 main-stem sites, 10 drain sites, and 2 sites at the discharges of wastewater-treatment plants. Three samples are included in both the time-series and irrigation-run events. Phase two, conducted in January 1995 during the low-flow non-irrigation season, consisted of a non-irrigation synoptic sampling event during which 18 water-column samples were collected at seven main-stem sites, nine drain sites, and two sites at the discharges of wastewater-treatment plants and a bed- material sampling event during which 6 bed-material samples were collected at six sites near the mouths of drains that discharge to the Rio Grande. The 51 water-column samples were analyzed for 78 pesticides and metabolites and 8 nutrients along with other constituents. The six bed-material samples were analyzed for 21 pesticides and metabolites, gross polychlorinated biphenyls, and gross polychlorinated naphthalenes. The presence of dissolved pesticides in the surface water of the Mesilla Valley is erratic. A total of 100 detections of 17 different pesticides were detected in 44 of the water-column samples. As many as 38 percent of these detections may be attributed to pesticide use upstream from the valley or to nonagricultural pesticide use within the valley. There were 29 detections of 10 different pesticides in 17 samples during the irrigation run and 41 detections of 13 pesticides in 16 samples during the non-irrigation run. Nine pesticides were detected during both phases of the study. The most commonly detected pesticides in the water-column samples were DCPA, which was detected in 29 samples, and metolachlor, which was detected in 17 of the samples. DCPA was detected throughout the Mesilla Valley, whereas metolachlor was detected mainly in the northern and central parts of the valley. The maximum pesticide concentration found during the study was 0.75 microgram per liter of carbofuran, which was detected at the East Side Drain site during the irrigation run. No water-column pesticide concentration exceeded U.S. Environmental Protection Agency's drinking-water standards or any applicable Federal or State criteria or guidelines. A total of 21 occurrences of six pesticides and metabolites were found in the bed-material samples. Chlordane, diazinon, and methyl parathion were detected once each, whereas DDD, DDE, and DDT were detected at all six bed-material sites. Water-column samples for the analysis of nutrient concentrations were collected at all sampling sites during both phases of the study. The concentrations of each nutrient ranged from at or below the individual minimum reporting level to as much as two or three orders of magnitude larger than the minimum reporting level. The concentration of each nutrient was left skewed with most of the values toward the lower end of the range. The larger concentrations of each nutrient, except dissolved nitrite plus nitrate, were associated with wastewater-treatment- plant sites 4 and 16. The larger concentrations of dissolved nitrite plus nitrate were generally associated with the non- irrigation run; however, the largest concentration was at site 4 during the irrigation run. During this study, the Mesilla Valley as a unit was a source of nutrients to the Rio Grande. Wi