title: Determination of traces of As, B, Bi, Ga, Ge, P, Pb, Sb, Se, Si and Te in high-purity nickel using inductively coupled plasma-optical emission spectrometry (ICP-OES).
abstract: A method has been developed for the determination of traces of arsenic, boron, bismuth, gallium, germanium, phosphorus, lead, antimony, selenium, silicon and tellurium in nickel matrix. The sample was dissolved in HClO4 (~ 150°C) and nickel was settled as crystalline nickelperchlorate [Ni(ClO4)2] on cooling. The mixture was ultrasonicated and after the separation of Ni(ClO4)2, analytes of interest were determined in the supernatant using ICP-OES. Similarly, it was also found that, after the dissolution of nickel in perchloric acid, when the solution temperature was maintained at ~ 100°C, long needle like crystals of nickel perchlorate were formed. The crystals were separated from the mixture and trace elements in the supernatant were determined using ICP-OES. In both methods the matrix removal was >99% and the recoveries of analytes were in the range 92-97%. The limits of detection for As, B, Bi, Ga, Ge, P, Pb, Sb, Se, Si and Te were found to be 0.18, 0.21, 0.07, 0.06, 0.25, 0.11, 0.09, 0.10, 0.17, 0.20 and 0.07 μg g(-1) respectively. The procedure was applied for the analysis of a standard reference material nickel oxide (SRM 761, Nickel Oxide No.1, NBS, USA) and the values obtained are in close agreement with the certified values.
authors.affiliation: National Centre for Compositional Characterization of Materials, Bhabha Atomic Research Centre, ECIL-Post, Hyderabad-500062, India.
authors.forename: S
authors.initials: S
authors.lastname: Thangavel
authors.affiliation: National Centre for Compositional Characterization of Materials, Bhabha Atomic Research Centre, ECIL-Post, Hyderabad-500062, India.
authors.forename: K
authors.initials: K
authors.lastname: Dash
authors.affiliation: National Centre for Compositional Characterization of Materials, Bhabha Atomic Research Centre, ECIL-Post, Hyderabad-500062, India.
authors.forename: S M
authors.initials: SM
authors.lastname: Dhavile
authors.affiliation: National Centre for Compositional Characterization of Materials, Bhabha Atomic Research Centre, ECIL-Post, Hyderabad-500062, India. Electronic address: sahayamac@gmail.com.
authors.forename: A C
authors.initials: AC
authors.lastname: Sahayam
keywords: Impurities; Nickel; Nickel alloys; Nickel perchlorate