manual tuning and matching (T&M) yielded the certified purity value within 1% error. Employing the automatic 90PW calibration, EC-qHNMR with automatic vs. Automatic calibration of the 90° pulse width (90PW) formed the foundation for the principle of reciprocity and used optimized nutation experiments, showing good agreement with values derived from manual high-precision measurement of 360PW. To overcome this hurdle, this study applied the principle of reciprocity, certified reference materials (caffeine as analyte, dimethyl sulfone as calibrant), and a systematic evaluation of data acquisition workflows to extract key factors for the achievement of accuracy and precision in EC-qHNMR. While ideal for intrinsically mass-limited samples, external calibration (EC) qHNMR is overshadowed by the prevalence of internal calibration and perceived rather than real practical limitations. Quantitative 1H NMR (qHNMR) is a highly regarded analytical methodology for purity determination as it balances metrological rigor, practicality, and versatility well.
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