Selectlve solid-phase extraction from environmental waters of nlne popular acldlc herblcldes was accompllshed by using one mlniaturlzed cartridge contalning in the top slde 50 mg of a nonspecific adsorbent, that Is graphitized carbon black (Carbopack B), and In the lower side 70 mg of a slllca-based strong anlon exchanger (SAX). After sample percolation, the SAX materlai was actlvated by passlng through the trap sodlum acetate, l moi/L. A 3-mL solvent mlxture of CH, Ci , / CH, OH (80:20, by volume) badfled with 1 mmol/L NaOH was then allowed to flow through the cartridge, and phenoxy acids were removed from the Carbopack surface and selectively readsorbed on the exchanger surface. After washing, the nlne herblcides were desorbed from the SAX surface wkh 0.0 mL of water/methanol (50:50, by volume) contalning trlfluoroacetlc acid and potasslum chloride. A 100-pL portion of thls solution was directly injected into the HPLC column, operatlng in the Ion suppression-reversed-phase mode. As ion suppressor, the substitutlon of the commonly used acetlc acld with trlfluoroacetlc acid allowed sensitive detectlon at 230 nm. Recovery of the nlne acidic herblcides ranged between 94% and loo%, lrrespectlve of the sample type considered. By thls extractlon method, bask, neutral, and weakly acldic compounds do not interfere with the analysis. Interestlngly, thls cartridge Is suitable for fleld sampllng, as Carbopack is able to adsorb phenoxy aclds from water at whatever pH value. The llmlts of detectlon of the nlne herbicides were well below 0.1 pg/L. The effectiveness In terms of recovery and selectivity of the two-adsorbent tandem system was compared with that of a C-18 disposable cartrldge.In the last decade, as an alternative to liquid partitioning, the method of combined extraction and preconcentration of organic compounds in water by adsorption on proper solid materials followed by desorption with a small quantity of an organic solvent has been employed extensively for trace determination of contaminants in environmental waters (1-8). The recent availability of sorbents in small, inexpensive cartridges has contributed t o the dramatic expansion of the use of solid-phase extraction (SPE), as evidenced by some selected publications (9-13). Besides solving well-known problems associated with the classical solvent extractionsolvent removal method, the S P E technique is particularly attractive as it lends itself to coupling with chromatographic systems for on-line applications (14). Another impressive feature of the SPE technique is that small sorbent traps can be deployed in the field by using newly available submersible instrumentation (15,16). In this way, combined sampling, extraction, and preconcentration are done at the sampling site, thus eliminating most contamination and handling problems connected to the sample collection. In addition, immediate isolation of organics from the aqueous matrix by an adsorbing material can preserve analytes from bacterial attack occurring between the time of sample collection and analysis...