The assessment of nickel purity used in the preparation of Ni-based super-alloys has been carried out through multielemental analysis by Glow Discharge Quadrupole Mass Spectrometry. Relative Sensitivity Factor (RSF) values generated from certified iron matrix reference samples (NIST 1761 and 1762 low alloy steel) were found to be suitable for the computation of trace element concentrations. Different wet chemical procedures were also carried out for the determination of different trace element constituents of the sample. The GD-QMS results were compared with those obtained through wet chemical methods. The GD-QMS results are in good agreement with those obtained from wet chemical procedures. A better assessment of nickel metal purity was achieved through GD-QMS. A variety of molecular ions formed through the reaction of nickel (matrix) with the discharge gas (argon) and other elements were observed.