定量核磁共振氢谱测定氘代碘甲烷的氘代率

建立了测定氘代碘甲烷氘代率的定量核磁共振氢谱方法。实验以氘代二甲基亚砜（DMSO-d₆）为氘代溶剂、对苯二甲酸二甲酯为内标物，在400 MHz光谱仪上进行测定。选择谱宽4807.69 Hz，激发偏置为2000.65 Hz，弛豫延迟时间为65 s，扫描次数为16次，以二氘碘甲烷氢（δ2.16）为定量峰，对苯二甲酸二甲酯的苯环氢（δ8.07）为内标峰。对线性关系、精密度、重复性、稳定性及耐用性等进行了方法学评价，结果良好。表明定量氢核磁共振法可用于氘代碘甲烷的氘代率测定，该方法准确可靠，简便快捷，且无需自身对照品，能够满足实验室中氘代碘甲烷氘代率的检测。

Determination of deuteration rate of iodomethane-d3 using quantitative proton nuclear magnetic resonance

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.