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The combination of laser-induced breakdown spectroscopy (LIBS) and laser-induced fluorescence (LIF) was investigated to improve the limit of detection (LoD) of trace elements in liquid water, while preserving the distinctive on-line monitoring capabilities of LIBS analysis. The influence of the main experimental parameters, namely the ablation fluence, the excitation fluence, and the inter-pulse delay was studied to maximize the fluorescence signal. The plasma was produced by a 266 nm frequency-quadrupled Q-switched Nd:YAG laser and the trace elements under investigation were then re-excited by a nanosecond optical parametric oscillator (OPO) laser, delivering pulses in the sub-mJ energy range, and tuned to strong absorption lines of the trace elements. The reproducibility of the measurements was improved using a home-made flow-cell, and relative standard deviations as low as 6.7% for a series of 100 shots were attained with a repetition rate of 0.7 Hz. Using the LIBS-LIF technique, we demonstrated LoDs of 39 ppb and 65 ppb for Pb and Fe, respectively, accumulating over 100 laser shots only, which correspond to an improvement of about 500 times with respect to LIBS. [ABSTRACT FROM AUTHOR]

Abstract: The combination of the laser-induced breakdown spectroscopy (LIBS) and laser-induced fluorescence (LIF) techniques was investigated to improve the limit of detection (LoD) of trace elements in solid matrices. The influence of the main experimental parameters on the LIF signal, namely the ablation fluence, the excitation energy, and the inter-pulse delay, was studied experimentally and a discussion of the results was presented. For illustrative purpose we considered detection of lead in brass samples. The plasma was produced by a Q-switched Nd:YAG laser and then re-excited by a nanosecond Optical Parametric Oscillator (OPO) laser. The experiments were performed in air at atmospheric pressure. We found out that the optimal conditions were obtained for our experimental set-up using relatively weak ablation fluence of 2–3 J/cm2 and an inter-pulse delay of about 5–10 μs. Also, a few tens of microjoules was typically required to maximize the LIF signal. Using the LIBS–LIFS technique, a single-shot LoD for lead of about 1.5 part per million (ppm) was obtained while a value of 0.2 ppm was obtained after accumulating over 100 shots. These values represent an improvement of about two orders of magnitude with respect to LIBS. [Copyright &y& Elsevier]