Analysis of Ethylenediamines

Significance of Ethylenediamine Analysis

Ethylenediamines and related polyamines are key building blocks in petrochemical and polymer industries. Rapid and reliable quantification of these basic compounds is critical for quality control and process monitoring in chemical manufacturing.

Objectives and Overview

This study demonstrates a gas chromatographic method using an underivatized SH-5 Amine column to separate and detect seven amine compounds, including isopropanol, monoethanolamine, ethylenediamine, piperazine, diethylenetriamine, aminoethylethanolamine, and aminoethylpiperazine. The focus is on achieving sharp peaks, baseline separation, and short analysis times.

Methodology and Instrumentation

• Instrument: Gas chromatograph with flame ionization detector (FID).
• Column: SH-5 Amine, 30 m × 0.25 mm I.D., 0.50 μm film thickness.
• Oven program: 40 °C for 4 min, ramp 10 °C/min to 315 °C, hold for 5 min.
• Injection: 3 μL under split 1:20, injector at 315 °C.
• Carrier gas: Hydrogen at 43 cm/s (constant head pressure 8.7 psi).
• Detector settings: FID at 315 °C, sensitivity 6.4 × 10⁻¹¹ AFS, dead time 1.9 min.

Main Results and Discussion

The method provided complete separation of the target amines within 20 minutes. Baseline resolution (> 1.5) was attained for all pairs, and retention times were reproducible with relative standard deviations below 1 %. The optimized temperature program minimized peak tailing for polar amines without derivatization.

Benefits and Practical Applications

• Eliminates the need for derivatization, reducing sample preparation time.
• High resolution and reproducibility support routine QA/QC in chemical production.
• Applicable to monitoring amine levels in process streams, environmental samples, and finished products.

Future Trends and Potential Applications

• Integration with mass spectrometry for enhanced selectivity and identification.
• Development of stationary phases tailored for ultra-polar analytes.
• Automation and miniaturization for on-line process monitoring.

Conclusion

The GC/FID method using an SH-5 Amine column offers a fast, accurate, and straightforward approach to analyze underivatized ethylenediamines and related compounds, streamlining quality control workflows and supporting diverse industrial applications.

Reference

Shimadzu Corporation, ERAS-1000-0457, First Edition: Sep. 2023