Supported liquid membrane coupled on-line to potentiometric stripping analysis at a mercury-coated reticulated vitreous carbon electrode for trace metal determinations in urine

Abstract

A method for trace metal determinations in complex matrices is presented. The method combines supported liquid membrane (SLM) sample clean-up and enrichment with potentiometric stripping analysis (PSA) in a flow system using reticulated vitreous carbon (RVC) as the electrode material. The membrane contained 40% m/m di-2-ethylhexylphosphoric acid dissolved in kerosene. Lead was used as a model substance in high-purity water and urine samples. The samples were enriched after a simple pH adjustment. The SLM enrichment time was 10 min when the last 5 min electrodeposition on the RVC electrode at –1.0 V (versus Ag/AgCl) was performed simultaneously. The influence of various experimental parameters such as deposition time, deposition potential and flow rate on the lead signal was investigated. With a 10 min SLM enrichment including a 5 min deposition time, the detection limit for lead was 0.3 µg l^–1. The relative standard deviation for lead concentrations in the range 4–20 µg l^–1 was 0.05%. The overall SLM–PSA system was found to be stable for at least 100 urine analyses. The method was validated by running a reference urine sample. The result obtained (five replicates) was 9.7 µg l^–1 (standard deviation 1.8 µg l^–1) which is within the recommended range of 9.2–10.8 µg l^–1.