Total chloride in catalysts with Thermo Scientific ARL PERFORM’X Advanced WDXRF Spectrometer

Importance of the Topic

The quantification of chloride in alumina-supported catalysts is critical for evaluating catalyst performance, longevity and safety during production, regeneration and usage. Excess chloride can lead to corrosion and deactivation of catalytic sites, making reliable analytical methods essential in industrial and research laboratories.

Objectives and Study Overview

This study applies the UOP 979-02 method to determine total chloride in fresh, regenerated and spent alumina-supported catalysts using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry. The aim is to validate the ARL PERFORM’X spectrometer configuration in terms of precision, accuracy and speed of analysis.

Methodology and Instrumentation

Samples were ground to a fine powder and analyzed as loose powder under a helium atmosphere. Chlorine peak (Kα) scans identified optimal background positions for calibration.

• Instrument: Thermo Scientific ARL PERFORM’X WDXRF spectrometer
• X-ray tube: Rhodium anode, low current filament, 1500 W
• Optics: AX06 and Ge111 crystals, one collimator, one FPC detector
• Operating conditions: 30 kV, 50 mA, helium atmosphere
• Counting times: 60 seconds standard, 15 seconds for rapid analysis

Main Results and Discussion

Calibration employed linear regression of net Cl peak intensities versus known concentrations, yielding a standard error of estimation (SEE) of 0.013% over 0.2–2.9% Cl. Precision tests on a 1% Cl catalyst sample showed:

• SD = 0.002% at 60 s counting time
• SD = 0.004% at 15 s counting time

These results demonstrate excellent repeatability and accuracy suitable for routine analysis.

Benefits and Practical Applications of the Method

The methodology delivers rapid, precise and accurate chloride measurements with minimal sample preparation. Its robustness and flexibility support quality control in catalyst manufacturing, regeneration processes and research environments.

Future Trends and Opportunities

Advancements may include detector and crystal upgrades to extend the elemental range from beryllium to trans-uranics, further reduction of analysis times and integration with automated sample handling. Enhanced software features can facilitate in-line process monitoring and data analytics.

Conclusion

The ARL PERFORM’X WDXRF spectrometer offers a reliable, high-performance solution for total chloride determination in alumina-supported catalysts. Both precision and accuracy meet industrial quality control needs, while user-friendly OXSAS software ensures streamlined operation throughout instrument lifetime.