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Precipitation hardened nickel-based Alloy 725 (UNS N07725) has been proven susceptible to hydrogen embrittlement in oil and gas production. Moreover, current standards cannot differentiate unequivocally between acceptable and affected microstructures, making the development of an appropriate quality control test a priority for the oil and gas industry. Recently, Alloy 725 failures were associated with the precipitation of nanoscale Cr- and Mo-rich phases at grain boundaries (GBs). Since these intergranular precipitates could lead to Cr- and Mo-depletion along the decorated GBs (i.e., sensitization), the double-loop electrochemical potentiokinetic reactivation (DL-EPR) test was explored as an alternative approach to detect affected microstructures. Herein, the DL-EPR technique was optimized for Alloy 725 by testing three types of samples with different degrees of sensitization, including a full GB-decorated microstructure that was shown prone to hydrogen embrittlement in oil and gas service. The optimized DL-EPR test conditions were 2 M HCl + 1 M H2SO4 + 10−4 M KSCN aqueous solution at 30 °C with a 1.667 mV s−1 scan rate and a vertex potential of Ecorr + 700 mV. Results were reproducible and consistent with the degree of GB decoration determined using metallographic methods. The test procedure developed herein could lead to the standardization of the DL-EPR method for Alloy 725.

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Cast and wrought Ni‐based superalloys are materials of choice for harsh high‐temperature environments of aircraft engines and gas turbines. Their compositional complexity requires sophisticated thermo‐mechanical processing. A typical microstructure consists of a polycrystalline γ‐matrix, strengthening Ni3(Al,Ti) γ′ precipitates, carbides (MC, M6C, and M23C6), borides (M2B, M3B2, and M5B3), and other inclusions. Microalloying additions of B, C, and Zr commonly improve high‐temperature strength and creep resistance, although excessive additions are detrimental. Grain boundary (GB) segregation may improve cohesion and displace embrittling impurities. Finely dispersed carbides and borides are desired to control grain size via GB pinning. However, excessive decoration of GBs may lead to failure during processing and in‐service. Hence, a systematic review on the roles of B, C, and Zr in cast and wrought Ni‐based superalloys is required. The current state of knowledge on GB segregation and precipitation is reviewed. Experimental and modeling results are compared across various processing steps. The impact of GB precipitation on mechanical properties is most well researched. Co‐precipitation in proximity to GBs interacting with local microstructure evolution and mechanical properties remains less explored. Addressing these gaps in knowledge allows a more complete understanding of processing–microstructure–properties relationships in advanced cast and wrought Ni‐based superalloys.