Analytical Sciences

Abstract − Analytical Sciences, 34(6), 693 (2018).

Quantitative Analysis of Major and Minor Elements in Lead-free Solder Chip by LA-ICP-MS
Koyo IDO,*1,*2 Hideyuki OBAYASHI,*3,*4 Yanbei ZHU,*1 Takafumi HIRATA,*3 Akiko HOKURA,*2 Naoko NONOSE,*1 and Kazumi INAGAKI*1,*2
*1 National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563, Japan
*2 Graduate School of Engineering, Tokyo Denki University, 5 Senju Asahi-cho, Adachi, Tokyo 120-8551, Japan
*3 Geochemical Research Center, The University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033, Japan
*4 Laboratory for Planetary Sciences, Kyoto University, Kitashirakawa Oiwakecho, Sakyo, Kyoto 600-8502, Japan
A method was established for the quantitative analysis of the elements (Cu, Ag, Pb, and Sn) in solder samples by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), with Sn-based matrix matched standard solutions for defining the calibration curves. It was found that chloride-ion presented in commercially available Sn standard solution resulted in a precipitation of AgCl and caused the deterioration of the linearity of the calibration curve for Ag. Therefore, a laboratory-made chloride-free Sn solution was used to prepare Sn matrix matched standard solutions so as to ensure the stability of the elements including Ag. For the quantitative analysis of solder samples by LA-ICP-MS, the operating conditions of the LA instruments were set to obtain a fluence of over 12 J cm−2. This is mainly because of larger LA-induced elemental fractionations using a fluence of <10 J cm−2. The results for Ag, Cu, Pb, and Sn in a certified reference material (NMIJ CRM 8203-a) were close to, or in agreement with, the certified values, indicating that the present method was valid for the quantitative analysis of the elements in solder samples. In comparison to the certified values, relatively larger uncertainties were obtained for the analytical results by LA-ICP-MS, which could be attributed to the dependence on the homogeneity of the sample because the sample aliquots used for analysis were much smaller than those required for the traditional analytical procedures (i.e., sample quantity ratio of ca. 1:13000). Further improvement of the uncertainty might be obtained by using a larger sample quantity for the analysis by LA-ICP-MS so as to improve the representativeness of the sample.