Simultaneous Analysis of Trace and Major Elements in Iron and Steel by ICPE-9820

Importance of the Topic

Iron and steel are fundamental materials in diverse industries, requiring precise control of elemental composition across a wide concentration range (ppm to tens of percent). High sensitivity and broad dynamic range are essential for accurate quality assurance and process control.

Objectives and Study Overview

This study evaluates the Shimadzu ICPE-9820 dual observation (axial/radial) ICP-AES for simultaneous determination of trace and major elements in various iron and steel certified reference materials, exploring its performance in terms of accuracy, sensitivity, and efficiency.

Methodology and Instrumentation

• Sample Preparation: Dissolution of 1 g samples in aqua regia, filtration, alkali flux fusion, combination, Y internal standard (100 mg/L), and dilution to 200 mL.
• Calibration: Matrix-matched high-purity Fe solutions spiked stepwise for multi‐range calibration curves.
• Instrumentation: Shimadzu ICPE-9820; RF power 1.2 kW; plasma gas 14 L/min; auxiliary gas 1.2 L/min; carrier gas 0.7 L/min; nebulizer with cyclone mist chamber; high-salt torch; axial and radial observation; ~3 min 40 s analysis per sample including rinse.

Key Results and Discussion

The system exhibited minimal memory effects (<0.016 mg/L for Ni/Cr) when alternating between high- and low-concentration samples. Calibration curves for Ni and Cr demonstrated excellent linearity (r > 0.9999) across multiple ranges without sample changes. Analytical values for Si, Mn, P, S, Cu, Ni, Cr, Mo, Ti, V, Nb, Al, Co, Sn, Zn, and Zr agreed with certified or high‐resolution ICP results, with detection limits down to 0.00001 wt%.

Benefits and Practical Applications

• Simultaneous trace and major element analysis streamlines workflow.
• Wide dynamic range eliminates repeated dilutions and reduces human error.
• Low memory effects ensure consistent accuracy across sequential measurements.
• Ideal for quality control and research in steel manufacturing.

Future Trends and Potential Applications

• Enhanced automation and software integration for real-time data evaluation.
• Application to more complex matrices such as advanced alloys and environmental samples.
• Faster sample introduction systems for reduced analysis time.
• Integration with high-resolution and multi-laser sources for improved detection of emerging trace elements.

Conclusion

The ICPE-9820 provides a robust platform for comprehensive elemental analysis in iron and steel, combining high sensitivity, broad dynamic range, minimal memory effects, and automated calibration selection, thus enhancing efficiency and reliability in industrial and research laboratories.

References

• JIS G1258-3:2014. Iron and Steel – ICP Atomic Emission Spectrometric Method – Part 3: Determination of Various Elements – Decomposition with Acids and Fusion with Sodium Carbonate.