Using high-performance quantitative NMR (HP-qNMR~?) for certifying traceable and highly accurate purity values of organic reference materials with uncertainties <0.1 %

摘要

Quantitative nuclear magnetic resonance (qNMR) in combination with metrological weighing is optimised to demonstrate the power of the qNMR measurement method. It is shown that with ~1H-qNMR it is possible to certify the purity of organic reference materials (expressed as mass fraction) with relative expanded uncertainties of <0. 1 % for a 95 % confidence interval (k = 2). Following well-defined selection criteria, a set of twelve different chemical compounds is evaluated and certified to serve as internal references for ~1H-qNMR measurements. A series of comparison measurements is made amongst a subset of the selected compounds. The purity of maleic acid is determined by six different ~1H-qNMR measurement series, and all results show full consistency. All the six mean values are covered within the range of ±0. 05 %. In two more measurement series, four different nuclei are analysed within the same sample against one calibrator. Even with non-optimised signal intensity ratios and varying signal pattern, a high consistency was obtained. Therefore, the validity and robustness of ~1H-qNMR measurement results are demonstrated. 1H-qNMR measurement results are directly traceable to a variety of internationally accepted primary reference materials, and therefore, traceability to SI units is obtained. All experiments are performed under ISO/IEC 17025 and ISO Guide 34 accreditation.