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• Highly sensitive and rapid Pb detection on modified nanomaterials in water samples. • Simultaneous preconcentration-determination by hyphenated flow injection-FAAS. • The nanomaterials were stable and reusable for ~350 cycles. • High sampling rate (~30 h−1) with excellent RSD (~1%) and accuracy (> 95%) values. • The recovery of Pb from contaminated water samples was > 95%. Lead contamination in drinking and natural water has reached alarming concentrations, thus necessitating the development of accurate and rapid determination systems for Pb(II) in aqueous systems. Two hyphenated flow injection-solid phase extraction- FAAS (FI-SPE-FAAS) systems using oxidized and m-phenylenediamine functionalized multiwalled carbon nanotubes for Pb(II) preconcentration from industrially contaminated real water samples have been proposed. The chemical and hydrodynamic parameters affecting Pb(II) sorption/desorption were optimized. The effect of common interfering ions in water was also studied. Different figures of merit such as preconcentration factor (> 70), detection limit (≤ 1.5 µg L−1), and relative standard deviation (≤ 1.3%) were achieved at the preconcentration time of 120 s for both the preconcentration systems. The method was applied to industrially contaminated real water samples and the spike recovery tests were carried out using standard Pb(II) solution traceable to NIST. The proposed method was validated using standard reference material 1640a supplied by NIST Gaithersburg, MD, USA. [ABSTRACT FROM AUTHOR]