Simultaneous in-line concentration for spectrophotometric determination of cations and anions

Abstract

A flow system is proposed for simultaneous in-line concentration of cations and anions. A sliding-bar commutator was employed to insert an anion and a cation exchange column into a flowing sample stream for serial retention of the analytes. In the injector alternative position, different solutions flowed through the columns for parallel elution of the species in different analytical paths. Three-way solenoid valves allowed the intermittent reagent introduction in the sample zones. Signals were measured by employing two flow-through LED-based detectors. The simultaneous retention of the sample zones in coiled reactors can be also performed to increase the residence time and the analyte conversion rate. The analytical potentiality was demonstrated by the in-line concentration of ammonium and phosphate followed by spectrophotometric detection. For a 90 s loading time, the sampling rate was estimated as 40 determinations per hour, which is three-fold higher than the obtained without performing the tasks simultaneously. Enrichment factors of 8.0 and 18 were estimated for phosphate and ammonium, respectively, yielding detection limits of 1 mg L-1 PO4(3-) and 1 mg L-1 NH4+ (99.7% confidence level). The reagent consumption was lower than 2 mg per determination. Results for freshwater samples agreed with the obtained by reference APHA procedures at the 95% confidence level.

Keywords

• flow-injection spectrophotometry
• multicommutation
• preconcentration
• phosphate
• ammonium