Direct determination of boron in Zr–2.5%Nb, Zr–1%Nb alloys and zirconium metals which are extensively used as structural materials in nuclear reactors has been carried out by glow discharge quadrupole mass spectrometer (GD-QMS). Relative sensitive factor (RSF) values for boron were determined using different solid standard reference mate-rials (Zircaloy and steel). A comparison of the GD-QMS results obtained using these RSF values, with DC–Arc-AES (direct current arc atomic emission spectrometry)/certified values showed reasonably good agreement in all the Zr-based materials analysed for boron in the range of 0.1–7 mg kg^-1. Quantitation of boron in Zr matrix is possible even with a steel standard when certified for Zr and B. Internal precision (intra-sample precision) was found to be typically ±4%RSD (relative standard deviation) and the inter-sample precision was ±10% RSD for boron at_˜0.1 mg kg^-1levels.The overall accuracy of the procedure was found to be ±8% at_˜0.5 mg kg^-1levels of boron using Zircaloy and steel standards. Under optimised experimental conditions the detection limit for boron was found to be ±13μgkg^-1.