Nitrosamines - Analysis of EPA 8270 nitrosamines

Significance of the Topic

Nitrosamines are potent carcinogens and environmental contaminants that require reliable monitoring at trace levels. Rapid, sensitive analysis is essential for water quality assessment, regulatory compliance, and public health protection.

Study Objectives and Overview

This application note describes a streamlined gas chromatography–flame ionization detection (GC-FID) method to separate and quantify nine nitrosamines defined under EPA Method 8270. The protocol targets efficient analysis with a 20-minute runtime on an Agilent VF-5ms wide-bore column.

Methodology and Instrumentation

• Chromatographic Conditions
  
  • Column: Agilent VF-5ms, 0.53 mm × 30 m, 0.5 µm film thickness (Part No. CP8974)
  • Oven Program: 40 °C (4 min hold) ramped at 10 °C/min to 270 °C
  • Carrier Gas: Hydrogen at 50 kPa
  • Injection: Split mode, 0.5 µL, split flow 100 mL/min
  • Detector: Flame ionization detector maintained at 300 °C
  • Analyte Load: Approximately 5 ng of each nitrosamine (0.2% solution)
• Target Analytes
  
  1. N-Nitrosodimethylamine
  2. N-Nitrosomethylethylamine
  3. N-Nitrosodiethylamine
  4. N-Nitrosopyrrolidine
  5. N-Nitrosodi-n-propylamine
  6. N-Nitrosomorpholine
  7. N-Nitrosopiperidine
  8. N-Nitroso-n-butylamine
  9. N-Nitrosodiphenylamine

Main Results and Discussion

The method achieves baseline separation of all nine nitrosamines within a 20-minute run time. Peak resolution is robust, with consistent retention times and sharp peak shapes. Repeatability studies indicate relative standard deviations below 5% for peak areas, confirming method precision. The hydrogen carrier gas reduced analysis time while maintaining chromatographic efficiency.

Benefits and Practical Applications

• Fast turnaround time supports high-throughput environmental monitoring.
• Simplified isothermal hold combined with a single ramp reduces method complexity.
• GC-FID offers cost-effective detection for laboratories without mass spectrometry.
• Applicable to drinking water, wastewater, and industrial effluent analysis.

Future Trends and Opportunities

• Integration with automated sample preparation for fully unattended workflows.
• Coupling with mass spectrometry for enhanced sensitivity and confirmation of trace-level nitrosamines.
• Development of micro-bore columns and faster temperature ramps to further shorten analysis time.
• Application to emerging nitrosamine analogues and transformation products.

Conclusion

The described GC-FID method provides a rapid, reliable, and cost-effective approach for analyzing nine EPA 8270 nitrosamines. Its robustness and ease of use make it suitable for routine environmental testing and regulatory compliance.

Reference

Agilent Technologies, Inc. Application Note A02252, October 2011.