Analysis of Low-level Polycyclic Aromatic Hydrocarbons (PAHs) in Rubber and Plastic Articles Using Agilent J&W DB-EUPAH GC column

Importance of the Topic

Polycyclic aromatic hydrocarbons (PAHs) are persistent organic pollutants with known carcinogenic and mutagenic properties. They can become entrapped in rubber and plastic matrices via extender oils used during manufacture. Regulatory bodies such as the US EPA and European Commission limit PAH content in consumer products, creating a need for highly sensitive, selective analytical methods to ensure compliance and protect public health.

Study Objectives and Overview

This application note presents a gas chromatography/mass spectrometry (GC/MS) method for the simultaneous determination of 20 PAHs—comprising 16 EPA‐priority compounds plus four additional markers—in rubber and plastic articles. The study evaluates chromatographic resolution, linearity, recovery, and compliance with relevant EU directives.

Methodology

• Sample preparation: Pieces of rubber or plastic (2–3 mm, 500 mg) were extracted in 20 mL toluene with ultrasonic agitation at 60 °C for 1 hour.
• Standards: Surrogate standard p-terphenyl-d14; internal standards naphthalene-d8, acenaphthene-d10, phenanthrene-d10, chrysene-d12, perylene-d12 at 500 µg/L.
• Calibration: Five-level calibration from 5 to 500 ppb with internal standards spiked at 500 ppb.

Used Instrumentation

• GC/MS system: Agilent 7890 GC coupled to 5975C series MSD and 7683 ALS.
• Column: Agilent J&W DB-EUPAH, 20 m × 0.18 mm × 0.14 µm.
• GC conditions: Splitless 1 µL injection, helium at 52 cm/s, oven ramp 120 °C to 300 °C with post-run at 320 °C.
• MS conditions: Electron ionization, SIM/Scan (50–450 amu), source 250 °C, quadrupole 180 °C.
• Miscellaneous: Long-life septa, deactivated splitless liners, and 5 µL syringe.

Main Results and Discussion

The DB-EUPAH column achieved baseline separation of all 20 target PAHs, including critical isomer pairs (phenanthrene/anthracene Rs=1.80; fluoranthene/pyrene Rs=16.1; benzo[a/e]pyrene Rs=2.82; benzo(b/j/k)fluoranthenes Rs≥1.41). Calibration curves exhibited excellent linearity (R²>0.998). Recoveries in spiked plastic and rubber samples at 100 ppb ranged from 73.5 % to 119.4 %, satisfying both US EPA and EU requirements.

Benefits and Practical Applications

• High sensitivity and selectivity for trace‐level PAH detection in complex matrices.
• Compliance with US EPA and EU directives for priority PAHs.
• Robust column performance at elevated temperatures with low bleed.

Future Trends and Application Possibilities

• Extension to other persistent organic pollutants and emerging contaminants.
• Coupling with high‐resolution MS for enhanced selectivity and confirmation.
• Automation and miniaturization of sample preparation for higher throughput.
• In‐line monitoring and QA/QC integration in manufacturing processes.

Conclusion

The described GC/MS protocol using the Agilent J&W DB-EUPAH column provides a reliable, high‐resolution approach for simultaneous analysis of multiple PAHs in rubber and plastic articles. Demonstrated performance in separation, linearity, and recovery supports its application in regulatory compliance and quality control labs.

References

1. Fetzer JC. The Chemistry and Analysis of the Large Polycyclic Aromatic Hydrocarbons. Polycyclic Aromatic Compounds. 2000;27:143. doi:10.1080/10406630701268255.
2. European Commission. Commission Recommendation 2005/69/EC. 15 November 2005.
3. Szelewski M. Full Scan Low Level Polynuclear Aromatic Hydrocarbon Analysis using the Agilent Technologies 6890/5973 GC/MSD. Agilent Technologies; publication 5989-0264EN.
4. Lynam K, Smith D. Polycyclic Aromatic Hydrocarbon Analysis Using an Agilent J&W DB-5ms Ultra Inert Capillary GC Column. Agilent Technologies; publication 5989-9181EN. July 2008.
5. Smith D, Lynam K. GC/MS Analysis of European Union Priority Polycyclic Aromatic Hydrocarbons using an Agilent J&W DB-EUPAH Column with a Column Performance Comparison. Agilent Technologies; publication 5990-4883EN. 2009.
6. Agilent Technologies. How confident are you with your separations of critical PAH isomers? Publication 5990-5551EN.