GPC/SEC with SDV Columns and 2-Methyltetrahydrofuran

Importance of the Topic

With growing emphasis on sustainability and green chemistry, replacing traditional petroleum-based eluents in GPC/SEC with renewable solvents enhances environmental compatibility and aligns analytical workflows with modern regulatory and corporate goals.

Objectives and Study Overview

This application brief evaluates 2-methyltetrahydrofuran (2-methylTHF) as a mobile phase for GPC/SEC analyses of nonpolar polymers. Key aims include demonstrating solvent compatibility with SDV columns, assessing chromatographic performance with standard polymers, and validating detection with a refractive index detector.

Applied Methodology and Instrumentation

Chromatographic separations were performed isocratically at 1 mL/min using 2-methylTHF. SDV columns in a high molecular weight combination provided a broad pore size range. Samples of polystyrene (PS) and polymethyl methacrylate (PMMA) standards were prepared at 1 mg/mL (0.5 mg/mL for >1 000 000 Da). Calibration employed Agilent ReadyCal kits. A refractive index detector and Agilent WinGPC software were used for data acquisition and analysis.

Instrumentation

• Pump: Isocratic, flow rate 1 mL/min, mobile phase 2-methylTHF
• Autosampler: Injection volume 20 µL
• Columns (8×50 mm precolumn; three 8×300 mm analytical columns): SDV 5 µm, pore sizes 1 000 Å, 100 000 Å, 1 000 000 Å
• Temperature: 23 °C
• Detector: Refractive index
• Calibration kits: Agilent ReadyCal PS and PMMA
• Software: Agilent WinGPC

Main Results and Discussion

Solvent exchange from THF to 2-methylTHF was seamless, with no loss in column efficiency or plate count. PS and PMMA standards exhibited excellent solubility and produced well-resolved, reproducible chromatograms. Overlays of three PS mixtures (Mp 474–2 520 000 Da) and three PMMA mixtures (Mp 800–2 200 000 Da) demonstrated consistent retention behavior and acceptable signal-to-noise ratios with RI detection.

Benefits and Practical Applications

• Sustainability: 2-methylTHF is biomass-derived, reducing reliance on petrochemicals.
• Compatibility: Worked effectively with standard SDV column ensembles and common polymer standards.
• Performance: Maintained high resolution and detection sensitivity comparable to THF.
• Operational ease: Direct solvent substitution without column conditioning issues.

Future Trends and Potential Applications

Continued exploration of bio-based solvents in chromatographic techniques may extend to polar or mixed-mode separations. Advances in column chemistries tailored for greener eluents and integration with advanced detectors (e.g., multi-angle light scattering, viscometry) will broaden applications in polymer science and quality control.

Conclusion

2-Methyltetrahydrofuran serves as an effective, sustainable alternative to THF in GPC/SEC workflows for nonpolar polymers. Its compatibility with SDV columns and RI detection supports robust, high-quality molecular weight analysis while advancing green analytical practices.

References

1. Pace V., et al. 2-Methyltetrahydrofuran (2-MeTHF): A Biomass-Derived Solvent with Broad Application in Organic Chemistry. ChemSusChem. 2012;5(8):1369–1379.