Accreditation and Quality Assurance

, Volume 9, Issue 1–2, pp 55–63 | Cite as

An uncertainty budget for the determination of the purity of glyphosate by quantitative nuclear magnetic resonance (QNMR) spectroscopy

  • Tareq Saed Al-Deen
  • D. Brynn HibbertEmail author
  • James M. Hook
  • Robert J. Wells
Practitioner’s Report


An uncertainty budget is presented for the results of measurements of purity of the agrochemical glyphosate using 1H and 31P quantitative nuclear magnetic resonance (QNMR) spectroscopy. The budget combines intralaboratory precision from repeated independent measurements of a batch, and other Type A and Type B effects. Consideration of correlation of uncertainties in ratios of mass determinations has been included. Expanded uncertainties of the purity for single determinations of purity by 1H and 31P QNMR are 0.66% and 0.82% (95% confidence interval, k=2), respectively.


Uncertainty budget Measurement uncertainty Method validation Quantitative nuclear magnetic resonance (QNMR) Glyphosate Agrochemicals 



The authors acknowledge useful suggestions from Mr. G. O’Donnell of Workcover Australia.


  1. 1.
    Rackham DM (1976) Talanta 23:269–274CrossRefGoogle Scholar
  2. 2.
    Shoolery JN (1977) Progress in NMR Spectroscopy 11:79CrossRefGoogle Scholar
  3. 3.
    Greenhalgh R, Shoolery JN (1978) Anal Chem 50:2039–2042Google Scholar
  4. 4.
    Maniara G, Rajamoorthi K, Rajan S, Stockton GW (1998) Anal Chem 70:4921–4928CrossRefGoogle Scholar
  5. 5.
    Al-Deen TS (2002) Dissertation, University of New South Wales, Sydney, AustraliaGoogle Scholar
  6. 6.
    Al-Deen TS, Hibbert DB, Hook J, Wells R (2002) Anal Chim Acta 474:125–135CrossRefGoogle Scholar
  7. 7.
    Janke H (1998) CCQM/98 98:1-12Google Scholar
  8. 8.
    Cheung RWJ (2001) Anal ChemGoogle Scholar
  9. 9.
    Wells R, Al Deen TS, Hook J, Hibbert DB (1999) 3rd Biennial Conference of the Metrology Society of Australia. Metrology Society of Australia, Sydney, AustraliaGoogle Scholar
  10. 10.
    Wells R, Al Deen TS, Hook J, Hibbert DB (2002) J Agric Food Chem 50:3366–3374CrossRefPubMedGoogle Scholar
  11. 11.
    Ahvazi BC, Crestini C, Argyropoulos DS (1999) J Agric Food Chem 47:190–201CrossRefPubMedGoogle Scholar
  12. 12.
    Vlahov GS, Simone N. (2001) Magn Resonance Chem 39:689–695CrossRefGoogle Scholar
  13. 13.
    Spyros AD (2000) J Agric Food Chem 48:802–805CrossRefPubMedGoogle Scholar
  14. 14.
    Rana FR, Mautone AJ, Dluhy RA (1993) Appl Spectrosc 47:1015–23Google Scholar
  15. 15.
    Nouri-Sorkhabi MH, Wright LC, Sullivan DR, Kuchel PW (1996) Lipids 31:765–770PubMedGoogle Scholar
  16. 16.
    Paulsen PJ, Cooke WD (1964) Anal Chem 3:1713–1721Google Scholar
  17. 17.
    El-Tahtawy A, Wolf W (1991) Cancer Res 51:5806–5812PubMedGoogle Scholar
  18. 18.
    Green NA, Meharg AA, Till C, Troke J, Nicholson JK (1999) Chemosphere 38:1085–1101CrossRefPubMedGoogle Scholar
  19. 19.
    Mazzoni V, Bradesi P, Tomi F, Casanova J (1997) Magn Resonance Chem 35:81–90CrossRefGoogle Scholar
  20. 20.
    Vlahov G (1998) Magn Resonance Chem 36:359–362CrossRefGoogle Scholar
  21. 21.
    Lee KB, Kweon J, Jinlee H, Park H (1996) Polymer J 28:696–702Google Scholar
  22. 22.
    Henderson TJ (2002) Anal Chem 74:191–198CrossRefPubMedGoogle Scholar
  23. 23.
    Zyta Z, Pawel K, Jolanta H, Granzyana W (2001) J Pept Sci 7:466CrossRefPubMedGoogle Scholar
  24. 24.
    Jakeman DL, Mitchell DJ, Shuttleworth WA, Evans JNS (1998) J Biomol NMR 12:417CrossRefPubMedGoogle Scholar
  25. 25.
    Derome AE (1989) Modern NMR techniques for chemistry research. Pergamon, Elmsford, NYGoogle Scholar
  26. 26.
    EURACHEM (2000) Quantifying uncertainty in analytical measurement. EURACHEM, LondonGoogle Scholar
  27. 27.
    ISO (1995) Guide to the expression of uncertainty in measurement. International Organization for Standardization (ISO), GenevaGoogle Scholar
  28. 28.
    Hibbert DB (2003) Accred Qual Assur 8:195–199CrossRefGoogle Scholar

Copyright information

© Springer-Verlag 2004

Authors and Affiliations

  • Tareq Saed Al-Deen
    • 2
  • D. Brynn Hibbert
    • 2
    Email author
  • James M. Hook
    • 1
  • Robert J. Wells
    • 3
  1. 1.NMR FacilityUniversity of New South WalesSydneyAustralia
  2. 2.School of Chemical SciencesUniversity of New South WalesSydneyAustralia
  3. 3.Bob Wells and AssociatesGordon Australia

Personalised recommendations