Analysis of Elements in Cement Using ICPE-9820

Importance of the Topic

Cement composition directly influences concrete performance, including setting time, strength development, and visual appearance. Monitoring major and trace elements assures product consistency and durability in construction applications.

Objectives and Study Overview

This study evaluates the capability of the Shimadzu ICPE-9820 simultaneous ICP atomic emission spectrometer for multi-element analysis in Portland cement and blended cement (slag and fly ash). Samples are pretreated by alkali fusion following the Japan Cement Association standard method JCAS I-52-2000 to achieve complete dissolution of refractory oxides.

Methodology and Instrumentation

A summary of the analytical workflow and instrument settings is provided below:

• Sample Preparation: 0.2 g cement is dissolved in HNO₃, filtered, ashed, and fused with lithium metaborate. The melt is dissolved, acidified, and diluted to 100 mL.
• Internal Standards: Yttrium and indium are added to all samples at constant concentrations for signal normalization.
• Instrument: Shimadzu ICPE-9820 featuring a vertically oriented plasma torch for high-salt matrices and a vacuum spectrometer for stable vacuum-UV measurements.
• Operating Conditions: RF power 1.20 kW; plasma gas 14 L/min; auxiliary gas 1.20 L/min; carrier gas 0.70 L/min; nebulizer (10 UES) with cyclone mist chamber; axial and radial observation modes.

Main Results and Discussion

Quantitative results for certified reference materials aligned with certified values within established uncertainties:

• JCA-CRM-1: CaO 65.27% vs. 65.21±0.10%; Fe₂O₃ 2.65% vs. 2.67±0.02%.
• SRM 1881a: CaO 57.72% vs. 57.58±0.34%; Fe₂O₃ 3.00% vs. 3.09±0.11%.
• Trace components (MgO, Na₂O, K₂O, TiO₂, P₂O₅, Mn, Sr, Cr₂O₃, ZnO) were also determined accurately.
• Spectral profiles (e.g., Ca at 317.933 nm, Ti at 337.280 nm, Mn at 257.610 nm) showed clear emission peaks without torch clogging.
• Calibration curves for Fe, Mg, and P demonstrated excellent linearity over the analytical range.

Benefits and Practical Applications

The combination of alkali fusion and the ICPE-9820 offers:

• High reliability in analyzing cement matrices with elevated salt levels.
• Efficient sample throughput for routine quality control and certification.
• Cost-effective vacuum-UV analysis without the need for high-purity purge gases.
• Applicability to research and development in cement and concrete formulations.

Future Trends and Potential Applications

Emerging directions to enhance cement analysis include:

• Automated sample handling for increased laboratory throughput.
• Extension to supplementary cementitious materials such as silica fume and metakaolin.
• Integration of chemometric tools for predictive quality assessment.
• Improved torch and detector designs for ultra-trace element detection.

Conclusion

The Shimadzu ICPE-9820, combined with standardized alkali fusion pretreatment, provides accurate, stable, and efficient multi-element determination in cement. Its advanced torch design and vacuum spectrometer expand analytical capabilities for routine QC and research.

Reference

• Japan Cement Association. JCAS I-52-2000 Quantitation Method for Trace Components in Cement by ICP Emission Spectrometry and Electrical-Heating Atomic Absorption Analysis.