A method has been developed for the separation of Pb from trace impurities such as Nb, Ni, Sb, Sn, Ta, and Ti for their determination in Pb, PbLi, and PbBi alloy samples. Lead was separated as chloride fluoride (PbClF) precipitate. The method also enables the determination of hydrolyzable elements which are otherwise not recovered. The separation of Pb was found to be 99.5%, whereas the recovery of impurities was in the 82-94% range. Matrix-free solutions were analyzed for Nb, Ni, Sb, Sn, Ta, and Ti by inductively coupled plasma optical emission spectrometry (ICP-OES). The method was applied for the analysis of Pb, PbLi, and PbBi alloy samples. Relative standard deviations were in the 1.8-10.2% range and the process blank levels were at the lower µg/g level.
EXPERIMENTAL InstrumentationAn inductively coupled plasma optical emission spectrometer Model No. JY-2000, equipped with a 40.68 MHz radio frequency generator, was used for these studies and determinations (Jobin Yvon, Horiba, France). The operating parameters used are listed in Table I.