Improving the quantitative analysis of cementitious materials by solid state NMR

• Applicants: Privatdozent Dr.-Ing. Frank Bellmann; Dr. Harald Hilbig; Professor Dr. Dietmar Stephan
• Subject Area: Construction Material Sciences, Chemistry, Building Physics
• Term: from 2021 to 2026
• Project identifier: Deutsche Forschungsgemeinschaft (DFG) - Project number 440340258

• Final Report Year: 2025

Final Report Abstract

It was the aim of the current research project to develop strategies for an improved quantitative analysis of cementitious materials by nuclear magnetic resonance, NMR. The analysis of silicon-containing clinker phases such as alite or belite by 29Si MAS NMR was modified by introduction of a standard-based procedure. Compared to the standard-free method, application of the standard-based approach can prevent overestimation of alite. The same method can be used to analyze the degree of hydration in samples containing alite and C-S-H. Analysis of aluminum-bearing phases such as slag or thermally activated clays by 27Al MAS NMR can be improved by addition of an internal standard material which allows a much faster extraction of quantitative information from the spectra. Reference materials were produced that can be supplied to other NMR labs interested in quantitative analysis of cementitious materials. Beyond the investigations to improve quantitative analysis in this research project, the participating labs have conducted other qualitative and quantitative studies using NMR which have benefited from the results obtained in this project.

Publications

• Evolution of the particle size distribution of tricalcium silicate during hydration by synchrotron X-ray nano-tomography. Cement and Concrete Research, 156, 106769.
  Neubauer, J.; Sowoidnich, T.; Valentini, L.; Schulbert, C.; Naber, C.; Rößler, C.; DaSilva, J. & Bellmann, F.
  
• Mechanisms of carbonation hydration hardening in Portland cements. Cement and Concrete Research, 152, 106687.
  Zajac, Maciej; Irbe, Linda; Bullerjahn, Frank; Hilbig, Harald & Ben Haha, Mohsen
  
• Effect of aluminum on the structure of synthetic alkali-silica gels. Cement and Concrete Research, 166, 107088.
  Krüger, Miriam E.; Heisig, Anne; Hilbig, Harald; Eickhoff, Henrik; Heinz, Detlef & Machner, Alisa
  
• About the Colloidal Nature and the Osmotic Potential of ASR Products. RILEM Bookseries, 25-34. Springer Nature Switzerland.
  Giebson, Colin & Seyfarth, Katrin
  
• Acid attack on hydrated cement: effect of organic acids on the degradation process. Materials and Structures, 57(4).
  Hilbig, H.; Gutberlet, T. & Beddoe, R. E.