Abstract: In this study, a quantitative proton nuclear magnetic resonance (qHNMR) method was proposed to determine the deuteration rate of iodomethane-d3.An experiment was conducted on a 400 MHz spectrometer using dimethyl terephthalate (DMT) and dimethyl sulfoxide (DMSO-d₆) as the internal standard reference and deuterated solvent, respectively. The following parameters were set: spectral width 4807.69 Hz, transmitter frequency offset 2000.65 Hz, relaxation delay time 65 s, and number of scans 16 times. The peak of δ2.16 in iodomethane-d2 and that of δ8.07 in dimethyl terephthalate were considered as the quantitative and internal standard peaks, respectively. The methodological assessment of linearity, precision, repeatability, stability, and durability was performed, and good results were achieved. The proposed qHNMR method can be used for determining the deuteration rate of iodomethane-d3. This method is accurate, reliable, simple, and fast and does not require its own reference substance. Thus, it can meet the test requirements of iodomethane-d3 deuteration rate in the laboratory.

Key words: iodomethane-d₃, deuteration rate, quantitative proton nuclear magnetic resonance