Analytical and Bioanalytical Chemistry

, Volume 407, Issue 11, pp 3103–3113 | Cite as

Purity assessment of organic calibration standards using a combination of quantitative NMR and mass balance

  • Stephen R. Davies
  • Kai Jones
  • Anna Goldys
  • Mahuiddin Alamgir
  • Benjamin K. H. Chan
  • Cecile Elgindy
  • Peter S. R. Mitchell
  • Gregory J. Tarrant
  • Maya R. Krishnaswami
  • Yawen Luo
  • Michael Moawad
  • Douglas Lawes
  • James M. HookEmail author
Research Paper
Part of the following topical collections:
  1. Reference Materials for Chemical Analysis


Quantitative NMR spectroscopy (qNMR) has been examined for purity assessment using a range of organic calibration standards of varying structural complexities, certified using the traditional mass balance approach. Demonstrated equivalence between the two independent purity values confirmed the accuracy of qNMR and highlighted the benefit of using both methods in tandem to minimise the potential for hidden bias, thereby conferring greater confidence in the overall purity assessment. A comprehensive approach to purity assessment is detailed, utilising, where appropriate, multiple peaks in the qNMR spectrum, chosen on the basis of scientific reason and statistical analysis. Two examples are presented in which differences between the purity assignment by qNMR and mass balance are addressed in different ways depending on the requirement of the end user, affording fit-for-purpose calibration standards in a cost-effective manner.


Quantitative NMR Calibration standards Purity assessment Mass fraction 



The authors acknowledge and thank Dr Jill Rogerson and Mr Michael Moir (NMI) for their valuable editorial assistance and to Mrs Hilda Stender (UNSW) for technical assistance with the running of samples.

Supplementary material

216_2014_7893_MOESM1_ESM.pdf (25 kb)
ESM 1 (PDF 24.5 kb)


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Copyright information

© Springer-Verlag Berlin Heidelberg 2014

Authors and Affiliations

  • Stephen R. Davies
    • 1
  • Kai Jones
    • 1
  • Anna Goldys
    • 1
  • Mahuiddin Alamgir
    • 1
  • Benjamin K. H. Chan
    • 1
  • Cecile Elgindy
    • 1
  • Peter S. R. Mitchell
    • 1
  • Gregory J. Tarrant
    • 1
  • Maya R. Krishnaswami
    • 1
  • Yawen Luo
    • 1
  • Michael Moawad
    • 1
  • Douglas Lawes
    • 2
  • James M. Hook
    • 2
    Email author
  1. 1.Chemical Reference MaterialsNational Measurement InstituteNorth RydeAustralia
  2. 2.NMR Facility, Mark Wainwright Analytical CentreUniversity of NSWSydneyAustralia

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