Analysis of Brominated Flame Retardants by GC/MS

Importance of the Topic

Brominated flame retardants such as polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls (PBBs) have been widely used in plastics to enhance fire resistance. With the EU RoHS directive coming into effect in July 2006, monitoring these compounds in electronic and electrical equipment is critical for regulatory compliance and environmental protection.

Study Objectives and Overview

This application note presents a GC/MS-based analytical workflow for the detection and quantification of PBDEs in standard mixtures and polystyrene samples. Key goals include demonstrating sensitivity in full-scan and selected ion monitoring (SIM) modes and establishing calibration strategies for Deca-BDE.

Methodology and Used Instrumentation

The method employs electron ionization (EI) with both scan and SIM acquisition to profile PBDE congeners. Sample preparation for plastics involves dissolution in tetrahydrofuran (THF), filtration, centrifugation, and splitless injection of 1 µL.

• Gas chromatograph: Shimadzu GCMS-QP2010
• Column: UA1(HT), 15 m × 0.25 mm I.D., 0.1 µm film
• Temperature program: 80 °C (2 min) to 360 °C at 20 °C/min, hold 2 min
• Injector temp: 300 °C; helium carrier gas 150 kPa
• MS interface temp: 350 °C; ion source 250 °C
• Scan range: m/z 50–1000 at 0.6 s/scan

Main Results and Discussion

Full-scan TIC of PBDE standards revealed clear peaks for penta-, octa- and deca-BDE congeners with characteristic M−2Br fragments. In a polystyrene extract containing 5 % Deca-BDE, nona-BDE impurities were detected. SIM mode enabled detection of Octa- and Deca-BDE at low levels (0.09 ng and 0.42 ng respectively) that were not visible in scan mode. A calibration curve for the Deca-BDE ion m/z 799.3 demonstrated linearity from 20 to 1000 pg with excellent correlation.

Benefits and Practical Applications

The described GC/MS approach delivers robust identification and quantitation of restricted PBDEs in polymer matrices. It supports quality control in manufacturing, RoHS compliance testing, and environmental screening for persistent organic pollutants.

Future Trends and Opportunities

Advancements in high-resolution MS and multidimensional chromatography may further improve congener separation and sensitivity. Automated sample preparation and data processing will streamline routine monitoring. Expanding libraries to cover novel flame retardant replacements will be essential as regulations evolve.

Conclusion

The Shimadzu GCMS-QP2010 method provides a sensitive and reliable platform for analyzing brominated flame retardants in plastics. Combining scan and SIM modes ensures comprehensive screening and low-level quantitation, facilitating regulatory compliance under RoHS.

References

• Shimadzu Corporation. Application News No. M231: Analysis of Brominated Flame Retardants by GC/MS.