Handbook of ICP-QQQ Applications using the Agilent 8800 and 8900

Importance of the Topic

Modern semiconductor, environmental and materials applications demand ultratrace, interference-free measurement of dozens of elements in challenging matrices. Triple quadrupole ICP-MS (ICP-QQQ) with MS/MS (tandem quadrupole) capability provides unprecedented control over spectral interferences and background signals. The Agilent 8800 and 8900 ICP-QQQ systems combine high sensitivity, versatile cell-gas chemistry, axial acceleration, and robust plasma performance to deliver detection limits in the sub-ppt to low-ppb range for elements traditionally difficult to analyze, such as phosphorus, sulfur, silicon, chlorine, and trace contaminants in high-purity process chemicals.

Objectives and Study Overview

– Introduce the principle and configuration of Agilent’s triple quadrupole ICP-MS instruments (8800, 8900) and their MS/MS functionality.
– Demonstrate interference removal strategies (on-mass and mass-shift modes) using cell gases (He, H2, O2, NH3) for key analytes.
– Apply ICP-QQQ to semiconductor-grade process chemicals (ultrapure water, hydrogen peroxide, hydrochloric and nitric acids, sulfuric acid, N-methyl-2-pyrrolidone, methanol, isopropyl alcohol), silicon wafer digests, high-silicon matrices, and organometallic solutions.
– Evaluate performance metrics: background equivalent concentration (BEC), detection limits (DL), linearity, stability, and spike recovery.

Methodology and Instrumentation

– Instrument: Agilent 8800/8900 ICP-QQQ in semiconductor and advanced configurations.
– Sample introduction: PFA-based nebulizers, Peltier-cooled quartz spray chambers, inert sample paths for organic solvents, optional m-lens for high-matrix tolerance.
– Plasma conditions: “Cool” plasma for low-matrix samples, high-power robust plasma for organics, acidic and silicon matrices.
– MS/MS operation: Q1 filters all ions except the target mass; the reaction/collision cell (ORS4) uses specific cell gases to convert or attenuate interferences; Q2 selects either the original analyte ion (on-mass) or the reaction product ion (mass-shift).
– Tuning: multi-tune methods enable automatic switching among no-gas, He collision, H2, NH3, and O2 reaction modes within a single sequence.

Main Results and Discussion

– Ultrapure water: 26 semiconductor-critical elements in 0.1% HNO3 acidified ultrapure water measured at BECs < 0.5 ppt (50 ppt for B) and DLs < 0.3 ppt, using MS/MS and optional m-lens under hot plasma.
– Hydrogen peroxide: 35% H2O2 assayed undiluted by MSA, achieving single-digit ppt DLs for 26 SEMI elements and RSD < 8% over 3.7 hr.
– Semiconductor acids: Sub-ppt quantitation of trace metals in 35% HCl and 20% H2SO4 (no pretreatment), resolving Cl- and S-based interferences by O2 and NH3 MS/MS modes.
– Organic solvents: Detection of P, S, Si, Cl at ppb to sub-ppb levels in NMP, methanol, IPA using H2, O2, NH3 MS/MS modes.
– Silicon matrices: 10 ppm and 100 ppm Si digests analyzed for 38 elements at ppt-level DLs and spike recovery 90–110% RSD < 6%.
– Nanoparticles: spICP-QQQ with Fast Time-Resolved Analysis quantified Au, Fe, Si, TiO2, Ag, Al2O3 NPs (10–200 nm) in TMAH and organic reagents. Rapid multi-element spICP-QQQ mode profiled 5 NP types in <6 min.
– Hydride-gas contaminants: GC-ICP-QQQ achieved 0.01–1.8 ppb DLs for P, As, Si, Ge, S hydrides in arsine and other hydride gases, single injection, multi-tune acquisition.
– Materials analysis: O2 MS/MS and NH3 on-mass modes removed polyatomic MH+ and MO+ interferences to measure trace As in Co matrix (BEC 0.33 ppb) and trace REEs in high-purity REE oxides at ppt levels.

Benefits and Practical Applications

– Unmatched interference removal: MS/MS mass-shift and on-mass modes eliminate both polyatomic and isobaric overlaps.
– Lowest detection limits: Sub-ppt to low-ppb DLs for critical analytes in complex matrices.
– Broad multi-element coverage: Single-method acquisition for >40 elements and multiple sample types.
– Improved stability: High-power cool plasma and m-lens for high-matrix tolerance and signal robustness.
– Automated workflows: Single multi-tune method, integrated GC and spICP-QQQ modes, and automated standard addition systems reduce manual handling and contamination risk.

Future Trends and Potential Uses

– Expansion of GC/LC-ICP-QQQ for organic and speciation analyses in pharmaceuticals, food, and environmental sectors.
– Further development of spICP-MS/MS for characterization of emerging nanomaterials in complex industrial matrices.
– Integration of automated, in-line calibration and enrichment systems to enable high-throughput, contamination-controlled ultratrace analysis.
– Adoption of AI-driven optimization and real-time spectral deconvolution for method development and routine QC.

Conclusion

Agilent triple quadrupole ICP-MS instruments, with their MS/MS capability and versatile cell-gas chemistries, have established new benchmarks for ultratrace analysis in demanding applications. From semiconductor process chemicals, high-matrix silicon digests, and high-purity REE oxides to nanoparticle characterization and hydride gas impurities, ICP-QQQ consistently delivers sub-ppt to low-ppb detection limits and robust interference removal. The combination of multi-tune acquisition, high-energy cool plasma, optional m-lens, and automated sample handling provides a comprehensive solution for manufacturers, research laboratories, and QA/QC analysts seeking the highest confidence in ultratrace elemental analysis.

References

1. Technical Overview: Agilent 8900 Triple Quadrupole ICP-MS, Agilent publication 5991-6942EN.
2. Applications of ICP-QQQ: “Handbook of ICP-QQQ Applications,” 5th Edition, Agilent publications.
3. Ultra-trace Analysis of Semiconductor Reagents: Agilent publications 5991-5372EN, 5991-7701EN.
4. Nanoparticle Analysis by spICP-QQQ: Agilent publication 5994-0987EN.
5. GC-ICP-QQQ for Hydride Gases: Agilent publication 5991-5849EN.