A spark discharge system was coupled to laser-induced breakdown spectroscopy (SD-LIBS) to improve sensitivity in the determination of P in fertilizers. A LIBS system consisting of a Q-switched Nd:YAG laser operating at 1064 nm and emitting pulses at 50 mJ with a fluence of 70 J cm −2 at the focal point was used. Results of preliminary experiments suggested that the most appropriate wavelength to measure P was the P (I) line at 214.9 nm, which did not show interferences by Fe, Cu and Zn. The electrical discharge was provided by a homemade highvoltage electronic circuit consisting of two cylindrical tungsten electrodes at the optimized output voltage of 4.5 kV, with tips arranged at the optimal distances of 4 mm between them and 2 mm above the sample surface. To minimize the expected matrix effects calibration standards of P 2 O 5 in the range of 4.8 and 33.3% were prepared by mixing various amounts of a phosphate rock reference material (SRM-120c) with a mixture of CaCO 3 , CaSO 4 , (NH 2 ) 2 CO and KCl at a 1:1:1:1 mass ratio. The calibration curves obtained at a 4.5 kV SD-LIBS output voltage showed correlation coefficients ≥0.993, RSD ≤8% and LOQ 5.3% (m/m) P 2 O 5 . Data obtained by analyzing commercial samples by the proposed system were in good agreement, at 95% confidence level, with those obtained by using high-resolution continuum-source flame atomic absorption spectroscopy.

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