Introducing the EDXIR-Holder: Sample Holder/Stocker for Contaminant Measurement

Importance of the Topic

Combining energy‐dispersive X-ray spectroscopy and Fourier transform infrared spectroscopy enables rapid, nondestructive analysis of both inorganic and organic contaminants. This integrated approach is vital for quality control, production line monitoring, and forensic investigations.

Objectives and Study Overview

This work introduces the EDXIR-Holder, a novel sample holder designed to simplify and accelerate contaminant analysis by facilitating both EDX and FTIR measurements within a single fixture. Its performance is demonstrated using real production line contaminants.

Methodology and Instrumentation

The EDXIR-Holder is a compact, openable case measuring approximately 5 cm by 5 cm when closed. It features a dual film design with a 35 μm acrylic adhesive layer for sample attachment and a 5 μm polypropylene film optimized for X-ray transmission. A writable white frame allows sample identification. Samples are adhered and analyzed by pressing the ATR prism directly onto the adhesive layer for FTIR, and then closing the case to perform EDX with the polypropylene side facing the X-ray source.

The following instruments and conditions were employed

• EDX system EDX-8000 with Rh target X-ray tube. Voltage and current set to 15 kV for low‐atomic number elements and 50 kV for heavier elements in vacuum. Measurement diameter 1 mm. Integration times 30 seconds without filter and 60 seconds with filter.
• FTIR system IRAffinity-1S with MIRacle10 diamond ATR prism. Spectral resolution 4 cm-1, 40 scans, Happ-Genzel apodization, DLATGS detector.

Main Results and Discussion

FTIR analysis of a production line contaminant yielded an ATR spectrum matching a PVC formulation with phthalate ester plasticizer and calcium carbonate filler. EDX quantification confirmed major elements C2H3 (62.73%), Cl (25.14%), Ca (11.43%), and detected trace Pb (0.60%), Ti, Cr, Sr and Cu.
For thin polyethylene film samples, initial FTIR spectra were dominated by adhesive layer signals. Subtraction of the adhesive layer spectrum produced a clean PE spectrum, demonstrating the importance of difference analysis for small samples.

Benefits and Practical Applications

• Streamlined sample exchange and minimal handling reduce contamination risk and sample loss.
• Integrated storage within the holder ensures traceability and compact sample management.
• Combined EDX and FTIR in one fixture delivers comprehensive chemical and elemental characterization for industrial QAQC, environmental monitoring, and failure analysis.

Future Trends and Potential Uses

• Automation of holder handling for high‐throughput production line monitoring.
• Integration with advanced data analysis software for real‐time contaminant identification and reporting.
• Adaptation of the holder design for coupling with additional spectroscopic or microscopic techniques and microsampling workflows.

Conclusion

The EDXIR-Holder represents a versatile, user-friendly solution for combined EDX and FTIR contaminant analysis. It enhances laboratory efficiency and data reliability by minimizing handling steps and enabling rapid, nondestructive characterization of diverse sample types.

References

• Shimadzu Application News No. X255
• Shimadzu Application News No. A522A
• Shimadzu Application News No. A527