Analytica chimica acta · 2026
A novel HF free, rapid microwave-assisted vanadium-catalysed acid dissolution (MW-VCAD) of ceramic boron carbide (B4C) for the accurate and precise determination of trace metallic impurities and total boron using ICP-OES.
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Ankam Durga Prasad, Rastogi Lori, Dash K
Аннотация
BACKGROUND: Boron carbide (B4C) is an extraordinary ceramic material, known for its remarkable resistance to oxidation in air and chlorine gas even at 700 °C. This makes B4C extremely challenging to dissolve using wet chemical methods. This study, for the first time presents a novel HF free, and rapid microwave-assisted vanadium-catalysed acid dissolution (MW-VCAD) method for the complete dissolution of B4C. The enhanced oxidative capacity of HClO4-H2O2-H2SO4 in the presence of V5+ catalyst ensured oxidation of B4C to H3BO3 with the assistance of microwave heating.
RESULTS: The optimized method enabled dissolution of ∼200 mg of B4C within 1 h under microwave heating at ∼220 °C and 60 bar. The detailed sequential evolution of the digestion mixture and method optimization, including evaluation of acid combinations, reagent concentrations, and microwave program parameters are presented. The influence of two critical factors viz. sample mass (50 - 300 mg) and particle size (D50 : 17 - 443 μm) on dissolution efficiency is also examined. The resulting digests were analysed for trace metallic impurities (Al, Ca, Cr, Co, Cu, Fe, Mg, Mn, Ni, Si, Ti, W, Zr) and total boron using ICP-OES. Method was validated using B4C CRM (ERM ED-102) and by comparison with Na2CO3 fusion. The obtained limits of quantification (1.5 - 30 mg kg-1) confirm the method's capability for impurity determination. Real sample analyses confirmed that the developed method is suitable for the determination of trace impurities and total boron in different grades of B4C.
SIGNIFICANCE: Both trace impurities and total boron can be determined with single dissolution method. Further, due to significantly less dissolution time and high sample throughput (8 samples/h) the developed method has strong potential to be used as a routine procedure in quality control and quality assurance of B4C for nuclear, aerospace, defense, and other advanced high-end applications.
RESULTS: The optimized method enabled dissolution of ∼200 mg of B4C within 1 h under microwave heating at ∼220 °C and 60 bar. The detailed sequential evolution of the digestion mixture and method optimization, including evaluation of acid combinations, reagent concentrations, and microwave program parameters are presented. The influence of two critical factors viz. sample mass (50 - 300 mg) and particle size (D50 : 17 - 443 μm) on dissolution efficiency is also examined. The resulting digests were analysed for trace metallic impurities (Al, Ca, Cr, Co, Cu, Fe, Mg, Mn, Ni, Si, Ti, W, Zr) and total boron using ICP-OES. Method was validated using B4C CRM (ERM ED-102) and by comparison with Na2CO3 fusion. The obtained limits of quantification (1.5 - 30 mg kg-1) confirm the method's capability for impurity determination. Real sample analyses confirmed that the developed method is suitable for the determination of trace impurities and total boron in different grades of B4C.
SIGNIFICANCE: Both trace impurities and total boron can be determined with single dissolution method. Further, due to significantly less dissolution time and high sample throughput (8 samples/h) the developed method has strong potential to be used as a routine procedure in quality control and quality assurance of B4C for nuclear, aerospace, defense, and other advanced high-end applications.