Journal
ACCREDITATION AND QUALITY ASSURANCE
Volume 18, Issue 2, Pages 91-98Publisher
SPRINGER
DOI: 10.1007/s00769-012-0944-9
Keywords
Quantitative NMR; qNMR; Purity determination; Traceability; Certification; Uncertainty; Organic reference materials; CRM
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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 H-1-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 H-1-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 H-1-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 H-1-qNMR measurement results are demonstrated. H-1-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.
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