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Structure analytical methods for quantitative reference applications

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Abstract

The analytical methods mass spectrometry, UV/Vis, IR, Raman, Fluorometry, XRD, Mössbauer, and NMR used to elucidate chemical structure are evaluated regarding their capabilities to be used as primary analytical techniques in quantitative measurements, considering the criteria in the CCQM definition of primary methods. This includes a review of the respective measurement equations, the evaluation of the measurement uncertainty, and a discussion of evidence for the “highest metrological level”, as obtained from intercomparisons in contest with other methods. It is shown that only few methods fulfill the CCQM criteria. Quantitative NMR spectroscopy is one of them and may be considered as a potential primary method as recommended by CCQM because of being free of empirical factors in the uncertainty budget.

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Notes

  1. Note to Eq. 19: Due to the fact that the spectra of the analyte A and the internal standard Std are processed and evaluated alike, errors may be correlated, and a covariance term may have to be included in the uncertainty budget [20].

  2. In the paper mentioned here [29] confusion arises with the formulas used to calculate the purity. It should be noted that the purity P and the purity factor f should be distinguished. Otherwise somewhere a factor of 100 is wrong as for instance in Eqs. 3 and 6. We would recomend to use the accepted symbols [30].

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Acknowledgement

The authors thank the Federal Ministry of Economics and Labour (BMWA), the German Federation of Industrial Cooperative Research Associations “Otto von Guericke” (AiF) and the German Research Association of Medicine Manufacturers (FAH) for supporting this work within the project AiF-No. 13843 N/1.

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Authors and Affiliations

  1. Federal Institute for Materials Research and Testing (BAM), Department Analytical Chemistry, Reference Materials, Richard-Willstaetter-Strasse 11, 12489, Berlin, Germany

    H. Jancke, F. Malz & W. Haesselbarth

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  1. H. Jancke
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  2. F. Malz
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  3. W. Haesselbarth
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Correspondence to F. Malz.

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Jancke, H., Malz, F. & Haesselbarth, W. Structure analytical methods for quantitative reference applications. Accred Qual Assur 10, 421–429 (2005). https://doi.org/10.1007/s00769-005-0004-9

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