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

Significance of the Topic

Contaminant analysis in production lines and laboratory environments requires rapid and nondestructive identification of both elemental and molecular residues. Combining energy dispersive X-ray spectrometry with Fourier transform infrared spectroscopy enables a comprehensive assessment of metal inorganic polymeric and organic substances with minimal sample preparation and damage.

Objectives and Overview

This article presents the design and application of the EDXIR-Holder a compact openable case that streamlines sample handling for contaminant measurement. The holder allows samples to be adhered to an acrylic adhesive film for analysis and then closed in the same chamber for elemental analysis without additional manipulation.

Methodology

The EDXIR-Holder comprises a 35 μm thick acrylic adhesive film bonded to a 5 μm polypropylene layer transparent to fluorescent X-rays. For FTIR analysis the case is opened and the ATR prism is pressed directly onto the adhered sample. For EDX analysis the case is closed and positioned with the polypropylene film facing the X-ray source. The recommended sample size ranges from 1.5 mm to 5.0 mm with thicknesses of 0.5 mm to 1.5 mm for EDX and 0.1 mm to 4.0 mm for FTIR and weights under 1 g. Care must be taken with small or protruding samples to avoid film puncture and spectral overlap from the adhesive layer. In such cases difference spectra between the sample and adhesive layer can be used.

Used Instrumentation

• EDX System: EDX-8000 with Rh X-ray tube 15 kV for light elements auto 50 kV for heavy elements vacuum atmosphere 1 mm measurement diameter up to 60 second integration time
• FTIR System: IRAffinity-1S with MIRacle10 diamond ATR prism 4 cm-1 resolution 40 scans accumulation Happ-Genzel apodization DLATGS detector

Main Results and Discussion

An unknown contaminant from a production line was analyzed using the EDXIR-Holder. FTIR ATR spectra indicated a mixture of polyvinyl chloride phthalate ester and calcium carbonate. EDX quantification confirmed chlorine at 25.14% calcium 11.43% and trace lead 0.60% along with titanium chromium strontium and copper. Lead detection highlighted the advantage of combined techniques since it was not observed by FTIR alone. A separate test with a small polyethylene film fragment first yielded an incorrect match to ethylene acrylic acid due to the adhesive layer. Using the difference spectrum approach correctly identified polyethylene demonstrating the importance of proper sample coverage or spectral subtraction for minute samples.

Benefits and Practical Applications

• Minimized sample handling reduces risk of loss and contamination
• Rapid switch between FTIR and EDX without transfer improves laboratory efficiency
• Nondestructive analysis preserves sample integrity for further testing or archiving
• Compact design allows sample labeling and storage within the holder
• Integration with EDXIR-Analysis software supports streamlined data processing

Future Trends and Potential Applications

Advancements may include development of alternative adhesive materials to reduce spectral interference automated sample exchange systems and integration with machine learning algorithms for real-time contaminant identification. Expansion to other spectroscopic methods such as Raman or X-ray imaging could further broaden forensic quality control and environmental monitoring capabilities.

Conclusion

The EDXIR-Holder represents an innovative tool for efficient combined FTIR and EDX analysis of contaminants. Its openable film design simplifies workflows reduces manual steps and enhances the reliability of trace elemental and molecular identification tasks. The holder is particularly recommended for use alongside dedicated analysis software to maximize laboratory productivity.

References

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