Phthalate Analysis Using an Agilent 8890 GC and an Agilent 5977A GC/MSD

Significance of the Topic

Phthalates are widely used plasticizers that can leach into the environment and pose health risks. Regulatory frameworks such as RoHS 2 and REACH limit their use in electronics, toys and childcare articles. Sensitive, reliable analytical methods are essential for screening and compliance testing of phthalates in consumer products.

Objectives and Study Overview

This work evaluates the performance of the Agilent 8890 gas chromatograph coupled to a 5977A GC/MSD with an Xtr source. Seven phthalates regulated under RoHS 2 and REACH were quantified over a dynamic range of 0.05 to 1 mg/L. The study also applies the method to three real-world samples—two pen caps and one electrical cable—to demonstrate its utility as a screening tool.

Methodology and Instrumentation

Sample preparation involved extracting 1 g of material with 40 mL of methylene chloride at 35 °C for 20 minutes under sonication. Extracts were filtered through a 0.45 µm PTFE syringe filter and transferred to deactivated glass vials.

• GC system: Agilent 8890 with a splitless inlet, Agilent J&W HP-5ms column (30 m × 0.25 mm, 0.25 µm), helium carrier at 1.0 mL/min.
• Oven program: 50 °C (1 min), 30 °C/min to 280 °C, then 15 °C/min to 310 °C (5 min hold).
• MS detection: Agilent 5977A GC/MSD in EI mode, synchronous SIM/Scan, Xtr source at 300 °C.
• Acquisition software: MassHunter GC/MS.

Results and Discussion

Calibration curves for all seven phthalates showed excellent linearity (R² > 0.99). Minimum detection limits (MDLs) ranged from 0.001 to 0.006 mg/L. Total ion current and SIM traces confirmed clear separation and identification of each compound. In real-world samples:

• Pen cap 1 and pen cap 2 contained trace levels of DIBP and DEHP, with other phthalates below the calibration range.
• The electrical cable contained all seven phthalates, with DEHP, DINP and DIDP at significant levels above the calibration range.

These results highlight the method’s sensitivity and its capability to screen consumer products for regulated phthalates.

Benefits and Practical Applications

The Agilent 8890/5977A GC/MSD platform offers high sensitivity, linear response and rapid analysis for phthalate screening. It is well suited for quality control, regulatory compliance, and environmental monitoring in laboratories handling consumer and electronic materials.

Future Trends and Applications

Advances may include more efficient sample preparation techniques for bulk and surface analysis, expanded compound libraries for emerging plasticizers, and integration with automated, high-throughput platforms. Additionally, coupling with high-resolution MS and alternative ionization sources could broaden applicability to complex matrices and trace-level screening.

Conclusion

The described GC/MSD method delivers reproducible, linear quantitation of seven regulated phthalates at sub-µg/L levels. Its demonstrated performance on real products confirms its value as a screening and compliance tool in analytical and regulatory laboratories.

References

• Commission Delegated Directive (EU) 2015/863 of 31 March 2015 amending Annex II to Directive 2011/65/EU on restricted substances.
• Corrigendum to Regulation (EC) No 1907/2006 (REACH) of the European Parliament and Council of 18 December 2006 concerning registration, evaluation, authorization and restriction of chemicals.