Metals Analyses of Portland and Blended Cement Via Microwave Digester and Inductively Coupled Plasma Technologies

Document Type : Research Paper

Author

Institute of Aquatic and Applied Sciences, Davao del Norte State College, Panabo City, Philippines.

Abstract

The method involves a sample preparation technique through microwave digestion to extract eight metals (Si, Al, Mg, Ca, Fe, Na, K, and Ti) in Portland (SRM 1888b) and Blended (SRM 1881a) cement traceable to NIST, followed by spectrometric detection and quantitation via the simultaneous system inductively coupled plasma-optical emission spectroscopy (ICP-OES). A 0.2-gram sample of the materials was prepared for closed-system digestion at 1200W. After digestion, solutions were diluted in 50-mL dedicated polypropylene laboratory ware (volumetric flasks) and analyzed. Accordingly, the dilution and calibration patterns were determined. The analyses were performed in five replicates.  The detections of Si, Al, Mg, Ca, Fe, K, and Ti following radial mode and Na via axial torch orientation gave satisfactory results.  Reproducibility studies were conducted, and ICP-OES configurations were established for each element. The method was developed based on its figures of merit.  The procedure was validated with exceptional performance, except that it was not robust at a higher sample mass.  Operational maintenance procedures were established when many samples were run. Measurement uncertainty estimation is recommended to identify the sources and effects of measurement errors.

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Main Subjects

References

  1. José N, Ahmed H, Miguel B, Luís E, Jorge de B. Magnesia (MgO) Production and Characterization, and Its Influence on the Performance of Cementitious Materials: A Review. Materials [Internet]. 2020 Oct 23;13(21):4752. Available from: https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7660681/. https://doi.org/10.3390/ma13214752
  2. ASTM C114-00. Standard Test Methods for Chemical Analysis of Hydraulic Cement.
  3. Bediako M, Amankwah EO. Analysis of Chemical Composition of Portland Cement in Ghana: A Key to Understand the Behavior of Cement. Advances in Materials Science and Engineering. 2015;2015:1–5. https://doi.org/10.1155/2015/349401
  4. [4] Gustavo González A, Ángeles Herrador M. A practical guide to analytical method validation, including measurement uncertainty and accuracy profiles. TrAC Trends in Analytical Chemistry [Internet]. 2007 Mar;26(3):227–38. Available from: https://www.sciencedirect.com/science/article/pii/S0165993607000118#. https://doi.org/10.1016/j.trac.2007.01.009
  5. Nayak A, Parui K, Sharma S, Ratha S. Study and Analysis of Atomic Spectra. International Journal of Scientific and Research Publications (IJSRP). 2020 Nov 24;10(11):946–55. https://doi.org/10.29322/ijsrp.10.11.2020.p10787
  6. Hou X, Amais RS, Jones BT, Donati GL. Inductively Coupled Plasma Optical Emission Spectrometry. Encyclopedia of Analytical Chemistry. 2016 Mar 9;1–25. https://doi.org/10.1002/9780470027318.a5110.pub3
  7. Sullivan MP, Holtkamp HU, Meier SM, Hartinger CG. The Analysis of Therapeutic Metal Complexes and Their Biomolecular Interactions. Elsevier eBooks. 2017 Jan 1;355–86. https://doi.org/10.1016/b978-0-12-803814-7.00010-1
  8. Iti S. ICP-OES: An Advance Tool in Biological Research. Open Journal of Environmental Biology. 2020 Dec 26;027–33. https://doi.org/10.17352/ojeb.000018
  9. Betz JM, Brown PN, Roman MC. Accuracy, precision, and reliability of chemical measurements in natural products research. Fitoterapia [Internet]. 2011 Jan;82(1):44–52. Available from: https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3026088/. https://doi.org/10.1016/j.fitote.2010.09.011
  10. Horwitz W. The Variability of AOAC Methods of Analysis as Used in Analytical Pharmaceutical Journal of AOAC INTERNATIONAL. 1977 Nov 1;60(6):1355–63. https://doi.org/10.1093/jaoac/60.6.1355
  11. McClure FD, Lee JK. Computation of HORRAT Values. Journal of AOAC International. 2003 Sep 1;86(5):1056–8. https://doi.org/10.1093/jaoac/86.5.1056
  12. AOAC Guidelines for Single-Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals (2012) Official Methods of Analysis, 19th Ed., Appendix K, AOAC INTERNATIONAL, Gaithersburg, MD.
  13. Moosavi SM, Ghassabian S. Linearity of Calibration Curves for Analytical Methods: A Review of Criteria for Assessment of Method Reliability. Calibration and Validation of Analytical Methods - A Sampling of Current Approaches [Internet]. 2018 Apr 25; Available from: https://www.intechopen.com/books/calibration-and-validation-of-analytical-methods-a-sampling-of-current-approaches/linearity-of-calibration-curves-for-analytical-methods-a-review-of-criteria-for-assessment-of-method. https://doi.org/10.5772/intechopen.72932
  14. Al-Hakkani MF. A rapid, developed and validated RP-HPLC method for determination of azithromycin. SN Applied Sciences. 2019 Feb 11;1(3).
  15. ‌Tome T, Žigart N, Časar Z, Obreza A. Development and Optimization of Liquid Chromatography Analytical Methods by Using AQbD Principles: Overview and Recent Advances. Organic Process Research & Development. 2019 Aug 14;23(9):1784–802. https://doi.org/10.1021/acs.oprd.9b00238
  16. Vander Heyden Y, Massart DL. Chapter 3 Review of the use of robustness and ruggedness in analytical Data Handling in Science and Technology. 1996;79–147. https://doi.org/10.1016/s0922-3487(96)80016-5
  17. Chen HY, Chen C. Evaluation of Calibration Equations by Using Regression Analysis: An Example of Chemical Analysis. Sensors [Internet]. 2022 Jan 7;22(2):447. Available from: https://pmc.ncbi.nlm.nih.gov/articles/PMC8780995/
  18. Clarice D.B. Amaral, Fialho LL, Felipe P.R. Camargo, Camillo Pirola, Nóbrega JA. Investigation of analyte losses using microwave-assisted sample digestion and closed vessels with Talanta. 2016 Nov 1;160:354–9.
  19. ‌Genovesi L. Considerations for optimizing an ICP sample introduction system. 2017 Dec 15.
  20. Barros AI, Pinheiro FC, Nóbrega JA. Calibration strategies to correct for matrix effects in direct analysis of urine by ICP-OES: internal standardization and multi-energy calibration. Analytical Methods. 2019;11(27):3401-3409. https://doi.org/10.1039/C9AY00907H
  21. Karlsson S, Andersson JT, Petersson P. Matrix effects in simultaneous microwave-induced plasma optical emission spectrometry: new perspectives on an old problem. Journal of Analytical Atomic Spectrometry. 2023;38(9):1983-1992. https://doi.org/10.1039/D3JA00061C
Journal of Chemical and Petroleum Engineering
Volume 60, Issue 1
June 2026
Pages 109-125

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History

  • Receive Date: 07 January 2025
  • Revise Date: 15 February 2026
  • Accept Date: 12 April 2026

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