ABSTRACT Coupling solid-phase extraction (SPE) to flow systems has promoted a synergistic development. Whereas SPE mechanization leads to improved precision and higher sample throughput, as well as diminishes systematic errors and contamination risks, analyte concentration and separation from the sample matrix provides a remarkable impact on detectability and selectivity in flow analysis. Historical aspects, main cornerstones, tips for system design, and recent applications are critically reviewed, in the context of analyte(s) separation/concentration, sample clean-up, and release of sorbed chemical species involving both packed (e.g. mini-columns, cartridges, and disks) or fluidized (e.g. beads and magnetic materials) particles. Novel (bio)sorbents, selective synthetic materials, and stationary phases for low-pressure chromatography are also discussed. Moreover, the feasibility of SPE for sample treatment before chromatographic separation, as well as the exploitation of direct measurements on the solid phase (optosensing) are emphasized.

Uma membrana tubular de PTFE permeável a espécies gasosas foi empregada como sonda em sistemas de análises em fluxo visando a proposta de uma estratégia de amostragem não invasiva. Como aplicação, foi selecionada a determinação espectrofotométrica de etanol em bebidas alcoólicas. A sonda é imersa na amostra, permitindo que o analito se difunda através desta e seja coletado pelo fluxo aceptor (solução ácida de dicromato), levando à formação de Cr(III), o qual é monitorado a 600 nm. Linearidade da curva analítica é verificada até 50,0% (v/v) de etanol (r > 0,998; n = 8), derivas de linha base são menores do que 0,005 absorbância durante períodos de 4 horas de operação e a velocidade analítica é de 30 h-1 o que corresponde a 0.6 mmol K2Cr2O7 por determinação. Os resultados são precisos (d.p.r. < 2%) e concordantes com aqueles obtidos por um método oficial.

A tubular gas diffusion PTFE membrane is exploited for non-invasive sampling in flow analysis, aiming to develop an improved spectrophotometric determination of ethanol in alcoholic beverages. The probe is immersed into the sample, allowing ethanol to diffuse through the membrane. It is collected into the acceptor stream (acidic dichromate solution), leading to formation of Cr(III), monitored at 600 nm. The analytical curve is linear up to 50% (v/v) ethanol, baseline drift is < 0.005 absorbance during four working-hours, and sample throughput is 30 h-1, meaning 0.6 mmol K2Cr2O7 per determination. Results are precise (r.s.d.< 2%) and in agreement with an official procedure.

The construction of a tubular hydrogen ion-selective potentiometric electrode without inner reference solution, based on the tridodecylamine (TDDA) ionophore, and its evaluation in a flow system are described. TDDA was dissolved in 2-nitrophenyl octyl ether, dispersed in a PVC membrane and applied directly to a conducting support which consisted of an epoxy resin and graphite mixture. The electrode was designed with a tubular geometry to effort facilities to be coupled as part of a flow injection network. The main working characteristics such as response time, linear pH range, selectivity and life time were evaluated and compared with those obtained which a conventionally shaped electrode based on the same sensor. The electrode showed a slope of 51-52 mV dec-1 within a linear pH range from 4.0 up to 12.0.