IntroductionRecently, environmental pollution by industrial waste has become a serious problem, and more rigorous environmental legislations have been enacted. In the European Union, for instance, the so-called "RoHS Directive" 1 regulated the use of six hazardous substances of lead (Pb), cadmium (Cd), mercury (Hg), hexavalent chromium (Cr(VI)), polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE) in new electrical and electronic equipment from July 2006. Therefore, an analytical method for rapid testing the materials and parts for the presence of these regulated substances is needed.Laser-induced plasma spectroscopy (LIPS) 2-4 is one of the suitable analytical methods for the RoHS directive, because of its capability of directly analyzing any type of material, including electrical non-conductors, without significant requirements of sample preparation. We studied the emission characteristics of the laser-induced plasma to improve the analytical performance, and showed the optimum conditions for quantitative analysis for non-conducting as well as conducting materials. [5][6][7][8][9][10][11][12][13] In our recent works, 14,15 we analyzed trace heavy metals of Pb, Cd, Hg and Cr in plastics by LIPS in argon at reduced pressure using time-resolved spectroscopy, and showed that these metal elements can be determined with detection limits of several tens ppm, and that the LIPS technique can be used for screening plastics for regulated elements.Currently, in accordance with the RoHS directive, lead-free solder has been used in the electronic assembly process, and verification of the lead-free nature of the solder is needed. Applications of Pb determination by LIPS were carried out by several researchers. For example, Castle et al. 16 analyzed Pb in paint samples using a portable LIPS instrument, but the detection limit obtained was relatively high (1200 ppm). Recently, Fornarini et al. 17 analyzed Pb in bronze samples in a relatively high concentration range of about 1 -10% by nanosecond laser-induced breakdown spectroscopy.The aim of the present work is to investigate the quantitative capability of LIPS for the determination of trace lead in leadfree solder, and to show that the LIPS method can be used for the in situ analysis and rapid screening of lead-free solder. For this purpose, the authors, with the use of a Q-switched Nd:YAG laser over a laser energy range of 10 to 90 mJ, analyzed commercially available lead-free solder certified reference materials in air at atmospheric pressure using time-resolved spectroscopy. The experimental results showed that a linear calibration curve was obtained for the analysis of lead in the concentration range from 174 to 1940 ppm by measuring spectra with a delay time of 0.4 μs after the laser shot at a laser pulse energy of 30 mJ.
ExperimentalThe experimental set-up used in this work is the same as that used in the analysis of plastic samples, 14,15 except for removing the optical windows of the sample chamber in order to analyze in air at atmospheric pressur...