Configuring the Dionex Integrion HPIC System for Trace Anion Determinations in Ultrapure Water

Importance of the Topic

Trace anion analysis in ultrapure water is essential for industries such as semiconductor manufacturing, power generation and electronics, where ppt-level contaminants can induce corrosion, reduce product yield and compromise process reliability. The Dionex Integrion HPIC system combined with automated sample preparation modules offers a robust platform to achieve ng/L–ppt sensitivity while minimizing baseline contamination and manual handling errors.

Objectives and Study Overview

This note presents a detailed workflow to configure the Thermo Scientific™ Dionex™ Integrion™ HPIC system with the Dionex™ AutoPrep™ module and Dionex™ EWP Electrolytic Water Purifier. The goals are to:

• Install and plumb the eluent generator, trap column, suppressor, autosampler and sample-preparation modules.
• Automate inline calibration and sample concentration for trace anion determinations.
• Demonstrate method performance (linearity, sensitivity, baseline stability) for fluoride, chloride, nitrite, bromide, nitrate, phosphate and sulfate in the 50–400 ppt range.

Methodology and Instrumentation

The system configuration includes:

• Eluent generation: Dionex EGC 500 KOH cartridge with CR-TC 600 trap column and high-pressure degasser (up to 5000 psi).
• Separation: Dionex IonPac AG17-C guard (4 × 50 mm) and AS17-C analytical column (4 × 250 mm) with 1.0 mL/min KOH gradient.
• Suppression: Dionex AERS 500e suppressor (4 mm, external water mode, 87 mA).
• Concentration: Dionex AutoPrep large loop (10 mL pull-mode) and small loop (10 µL) with valve switching managed by Chromeleon CDS.
• Carbonate removal: Dionex CRD 300 inline device prior to concentrator to eliminate CO₂ interference.
• Detection: Conductivity detection (CD) at 15 °C with tablet control and consumables monitoring.

The AutoPrep protocol uses a 1000× stock standard (50 mg/L) and multiple 10 µL injections to generate a 50–400 ppt calibration series, eliminating manual ppt-level standard preparation. Valve timing and overfill factors are empirically determined to ensure ≥10× loop overfill and reproducible transfers.

Main Results and Discussion

Calibration curves for chloride and sulfate exhibited r² ≥ 0.999 in the 50–400 ppt range; similar performance was observed for the other anions. The Dionex CRD 300 demonstrated superior carbonate removal compared to the CRD 200, ensuring negligible tailing and baseline drift (< 0.1 µS/min). Baseline contamination in system blanks ranged from 5 ppt (nitrate) to 13 ppt (nitrite, fluoride), yielding estimated 3× S/N detection limits of single- to double-digit ppt for all analytes.

Benefits and Practical Applications

• Closed-loop calibration and sample handling minimize environmental contamination.
• Automated inline dilution and concentration reduce labor and improve reproducibility at ppt levels.
• High-pressure eluent generation and integrated suppressor control deliver stable baselines and low detection limits.
• Consumables tracking and automated diagnostics enhance compliance and uptime.

Future Trends and Opportunities

Advances may include integration of AI-driven diagnostics for real-time system optimization, expansion to other trace analytes (cations, organics) and further miniaturization of fluidic pathways to reduce dead volume and sample consumption. Coupling with mass spectrometric detection or diode array opens multi-dimensional trace analysis workflows.

Conclusion

The Dionex Integrion HPIC system equipped with AutoPrep and EWP modules offers a turnkey solution for reliable ppt-level anion analysis in ultrapure water. Automated sample preparation, inline calibration and aggressive carbonate removal enable detection limits in the low tens of ppt while reducing user error and contamination risk. This configuration meets industry standards such as ASTM D 5127 for high-purity water quality control.

References

1. Christison T., Khor D., Moore D., Lopez L., Rohrer J. Configuring the Dionex Integrion HPIC System for Trace Anion Determinations in Ultrapure Water. Thermo Fisher Scientific Technical Note 177, 2016.
2. Thermo Fisher Scientific. Dionex AS-HV Autosampler Operator’s Manual (P/N 065259), 2012.
3. Thermo Fisher Scientific. Integrion HPIC Installation and Operator’s Manual (P/N 22153-97003), 2015.
4. Thermo Fisher Scientific. Eluent Generator Cartridges Product Manual (P/N 065018-05), 2014.
5. Thermo Fisher Scientific. Continuously Regenerated Trap Column (CR-TC) Product Manual (P/N 065018-05), 2012.
6. Thermo Fisher Scientific. ERS 500 Suppressor Product Manual (P/N 031956-09), 2013.
7. Thermo Fisher Scientific. IonPac AS17-C Column Product Manual (2014).
8. ASTM International. ASTM D 5127 Standard Guide for Ultra-Pure Water Used as a Solvent and Cleaning Agent in the Electronics and Semiconductor Industries, 2015.