A Matrix‐Corrected External PIGE Approach Using Synthetic Standards for Accurate Boron and Isotopic Ratio Measurements in Neutron‐Shielding Composites

The present study optimizes a simple, rapid, and nondestructive analytical methodology for the simultaneous determination of total boron concentration and its isotopic composition (IC) in Boron‐aluminum alloy and other boron‐containing neutron shielding materials widely used in nuclear reactors. External (in air) PIGE methodology, using prompt gamma rays from 181 Ta(p,p’γ) 181 Ta as a current normalizer, has been used. The report emphasizes the potential of the methodology for measuring 10 B/ 11 B atomic ratios in alloys using prompt gamma‐ray peaks at 429, 718, and 2125 keV corresponding to 10 B(p,αγ) 7 Be, 10 B(p,p’γ) 10 B, and 11 B(p,p’γ) 11 B nuclear reactions, respectively. The sensitivity of the gamma rays has been established using the synthetically prepared elemental standards for determining the total boron mass fraction in the alloy samples. The methodology has been applied to alloy and polymer‐based samples for the first time using nearly matrix‐matched synthetic standards. The uncertainty associated with the methodology has been evaluated along with the external precision of the samples. Moreover, quality assessment of the methodology was carried out in terms of t‐test and F‐test using alternate analytical techniques (mass spectrometry and titrimetry). The detection limit of boron in these shielding materials was found to be within (0.03–0.2)% using the optimized methodology.