Quantitative Analysis of Boron Trichloride Using ¹¹ B Quantitative Nuclear Magnetic Resonance Spectroscopy (qNMR)

Boron trichloride (BCl ₃ ) is highly reactive and degrades rapidly when exposed to moisture, complicating analyses, and posing safety risks under standard laboratory conditions. To address these challenges, quantitative ¹¹ B nuclear magnetic resonance (qNMR) spectroscopy has been introduced as an analytical method to accurately quantitate boron trichloride in solution. This technique involves the reaction of boron trichloride with methanol to produce trimethyl borate, which is then quantified using an external standard. The preparation process allows for the reaction and sample preparation to occur in a single step within the same vial, ensuring a safe, fast, and reliable analysis. The ¹¹ B qNMR method was validated, demonstrating linearity (0.02 M to 0.50 M with r  = 0.9999), accuracy (recovery of 100.05%), precision (inter‐ and intraday), stability, and robustness. This paper highlights the effectiveness of the ¹¹ B qNMR method for the accurate, reliable, fast, and safe quantification of boron trichloride in organic solvents such as dichloromethane.