Novel approach of qNMR workflow by standardization using 2H integral: Application to any intrinsic calibration standard

Quantitative nuclear magnetic resonance (qNMR) is routinely performed by the internal or external standardi-zation. The manuscript describes a simple alternative to these common workflows by using NMR signal of another active nuclei of calibration compound. For example, for any arbitrary compound quantification by NMR can be based on the use of an indirect concentration referencing that relies on a solvent having both 1H and 2H signals. To perform high-quality quantification, the deuteration level of the utilized deuterated solvent has to be estimated. In this contribution the new method was applied to the determination of deuteration levels in different deuterated solvents (MeOD, ACN, CDCl3, acetone, benzene, DMSO-d(6)). Isopropanol-d(6), which contains a defined number of deuterons and protons, was used for standardization. Validation characteristics (precision, accuracy, robustness) were calculated and the results showed that the method can be used in routine practice. Uncertainty budget was also evaluated. In general, this novel approach, using standardization by 2H integral, benefits from reduced sample preparation steps and uncertainties, and can be applied in different application areas (purity determination, forensics, pharmaceutical analysis, etc.).

Automated summary

This paper introduces a new method for quantitative nuclear magnetic resonance (qNMR) analysis, using the NMR signal of another active nuclei for calibration. The new approach can be used to determine deuteration levels in different deuterated solvents, with benefits of reduced uncertainties and sample preparation steps.