Agilent ICP-MS Journal (October 2020, Issue 82)

Significance of the Topic

High-sensitivity analysis of trace contaminants by ICP-MS and ICP-QQQ plays a critical role in industries ranging from semiconductor manufacturing to food safety. Precise quantification of hydride gas impurities in arsine precursors ensures performance and reliability of III-V compound semiconductors. In parallel, monitoring inorganic arsenic in infant rice cereals protects vulnerable populations and supports regulatory compliance. Advanced ICP-MS/MS methods also open new capabilities for challenging analytes like sulfur, while integrated software tools and webinars drive best practices and data quality improvements across routine and novel applications.

Objectives and Study Overview

This issue presents four key application areas:

• Development of a GC-ICP-QQQ method for sub-ppb measurement of silane, phosphine, hydrogen sulfide and germane impurities in arsine gas.
• Implementation of HPLC-ICP-MS protocols to comply with the new US FDA 100 µg/kg inorganic arsenic limit in infant rice cereal, including a rapid 2-minute screening approach.
• Insights from live webinars showcasing ICP-QQQ solutions for semiconductor process chemicals, nanoparticles and chlorine analysis in organic solvents.
• Accurate low-level sulfur determination by ICP-MS/MS with oxygen reaction cell gas and MS/MS filtering to overcome interferences.

Methods and Instrumentation

GC-ICP-QQQ study:

• Sample introduction via Agilent 7890B GC with high-flow Deans switch to vent matrix arsine post-elution.
• Detection on Agilent 8900 Triple Quadrupole ICP-QQQ operated in MS/MS mode with H₂ and O₂ cell gases and multi-tune acquisition.

HPLC-ICP-MS arsenic speciation:

• Isocratic anion-exchange separation of As(III), As(V), DMA and MMA on Agilent 1260 HPLC.
• Detection by Agilent 7900 ICP-MS following US FDA EAM 4.11 guidelines, with optional H₂O₂ oxidation for rapid iAs screening.

ICP-MS/MS sulfur analysis:

• O₂ reaction cell to generate SO⁺ product ions.
• MS/MS operation to exclude 32S precursor and measure 32S¹⁶O⁺ and 34S¹⁶O⁺ without overlapping interferences.

Semiconductor webinars:

• Single particle ICP-MS for Fe nanoparticles down to 15 nm at ppq levels.
• ICP-QQQ strategies for trace chlorine in organic matrices.
• Online sampling systems and automated standard addition workflows for gas and liquid process chemicals.

Used Instrumentation

• Agilent 7890B Gas Chromatograph
• Agilent 8900 Triple Quadrupole ICP-MS (ICP-QQQ)
• Agilent 1260 Infinity II LC
• Agilent 7900 Quadrupole ICP-MS

Main Results and Discussion

• GC-ICP-QQQ achieved detection limits of 0.01 ppbv for GeH₄ and ≤0.51 ppbv for other hydrides in arsine, enabling single-column, single-injection quantitation of four impurities.
• HPLC-ICP-MS iAs determination in six market rice cereals showed two samples exceeding the 100 µg/kg FDA action level, with relative standard deviations <5 % and low LOQs.
• Rapid 2-minute HPLC-ICP-MS screening delivered lower detection limits compared to standard FDA methods by pre-oxidizing As(III).
• Sulfur analysis by ICP-MS/MS produced accurate low-level S quantitation free from phosphorus and inter-isotope overlaps, extending ICP-MS utility for sulfur isotope and trace determination.
• Webinar case studies demonstrated robust control of metal nanoparticle and halogen impurities in semiconductor matrices, and the value of IntelliQuant and NebAlert software tools for real-time data quality monitoring.

Benefits and Practical Applications

• Enhanced semiconductor QC through precise hydride and nanoparticle impurity profiling supports device yield and reliability.
• Regulatory compliance for inorganic arsenic in infant foods, protecting consumer health and maintaining market access.
• Expanded analytical scope of ICP-MS to challenging elements such as sulfur, chlorine and fluorine via ICP-MS/MS, increasing lab capability with existing hardware.
• Improved data quality and troubleshooting using integrated software features to detect matrix suppression, interferences and abnormal nebulizer conditions in real time.

Future Trends and Applications

• Automation of gas and liquid sample introduction with online standard addition for improved accuracy and throughput.
• Wider adoption of single particle ICP-MS for nanoparticle characterization in high-purity process chemicals.
• Development of cloud-enabled AI tools for predictive maintenance and advanced interference correction.
• Further integration of triple quadrupole ICP-MS in environmental, life sciences and petrochemical analysis for elements previously inaccessible by single quadrupole instruments.

Conclusion

Agilent’s suite of ICP-MS and ICP-QQQ methods provides high-performance solutions for trace contaminant analysis across diverse fields, from semiconductor process control to food safety and challenging elemental determinations. Integration of advanced reaction cell chemistries, rapid chromatographic separations and real-time software diagnostics ensures accurate, reliable and efficient workflows that meet evolving regulatory and industrial requirements.

References

1. Geiger WM, McElmurry B, Anguiano J, Kelinske M. Agilent publication 5994-2213EN, 2020.
2. US FDA. Guidance for Industry: Action Level for Inorganic Arsenic in Rice Cereals for Infants, 2016.
3. US FDA. Elemental Analysis Manual Section 4.11: Arsenic Speciation in Rice and Rice Products Using HPLC-ICP-MS, 2018.
4. Juskelis R, Li W, Nelson J, Cappozzo JC. J Agric Food Chem. 2013;61(45):10670–10676.
5. Gray PJ, Tanabe CK, Ebeler SE, Nelson J. J Anal At Spectrom. 2017;32:1031–1034.
6. Tanabe CK, Ebeler SE, Nelson J. Agilent publication 5991-9488EN, 2017.