Automated Analysis of Semiconductor Grade Hydrogen Peroxide and DI Water using ICP-QQQ

Importance of the Topic

Maintaining ultralow levels of metallic and nonmetallic impurities in high-purity hydrogen peroxide and deionized water is critical to semiconductor yield and device performance. Even trace contaminants can degrade the electrical properties of wafers, making robust, sensitive analysis essential in every stage of production.

Objectives and Study Overview

This study presents an automated analytical workflow using an Agilent 8900 triple quadrupole ICP-MS coupled with the ESI prepFAST S system. It aims to quantify ultratrace elemental impurities in 35% H2O2 and DI water at part-per-trillion levels through online Method of Standard Additions calibration, minimizing manual handling and contamination risk.

Methodology and Instrumentation

Samples included high-purity hydrogen peroxide and Milli-Q water. A 1000 ng/L multi-element stock and a 10% HNO3 spike were automatically prepared by the prepFAST S system, which performed dilution, acidification, spiking, and calibration. The Agilent 8900 ICP-QQQ employed a PFA concentric nebulizer, a Peltier-cooled quartz spray chamber, quartz torch, platinum-tipped cones, and an s-lens. Collision/reaction gases (He, H2, O2, NH3) and cool plasma modes optimized interference removal and detection limits across 49 elements.

Main Results and Discussion

Automated MSA calibrations yielded linear response curves at ppt concentrations for major analytes (Na, K, Si, P, S, Ca, Zn, As). Detection limits below 1 ng/L were achieved for 46 elements in DI water and 45 in H2O2; only Si, P, and S required single-ppt levels. In DI water all elements were below detection limits except background equivalent concentrations for Si, P, and S (85, 10, and 118 ppt). In 35% H2O2 only B and Si exceeded 10 ppt, while P and S remained well below SEMI C30-1110 limits.

Benefits and Practical Applications

• Automated dilution, acidification, and calibration lower contamination risk and analyst time.
• Comprehensive coverage of all SEMI-specified elements, including challenging nonmetals, in a single run.
• Rapid, under-30-minute analysis with high throughput and reproducibility.
• Precision sample injection and high-speed rinsing ensure stable baselines and data quality.

Future Trends and Potential Applications

Further integration of inline automation with ICP-QQQ can enable real-time monitoring of process chemicals. Continuous advancements in reaction cell chemistry and software-driven tuning will extend detection capabilities for emerging contaminants. Adapting this workflow to other critical semiconductor reagents and broader manufacturing lines promises to enhance process control and yield optimization.

Conclusion

The combination of Agilent 8900 ICP-QQQ with ESI’s prepFAST S automation delivers a robust, sensitive, and efficient solution for ultratrace analysis of semiconductor-grade H2O2 and DI water. The system meets or exceeds SEMI Grade 5 specifications, reduces manual handling errors, and streamlines workflows, supporting the stringent contamination control demands of advanced semiconductor production.

Reference

1. SEMI C30-1110, Specifications for Hydrogen Peroxide, 2010.
2. Yamanaka K., Determination of Ultra Trace Elements in High Purity Hydrogen Peroxide with Agilent 8900 ICP-QQQ, Agilent Technologies, 2016, 5991-7701EN.
3. Nakano K., Ultra-Low Level Determination of Phosphorus, Sulfur, Silicon and Chlorine Using the Agilent 8900 ICP-QQQ, Agilent Technologies, 2016, 5991-6852EN.