FTIR talk letter (39)

Importance of the topic

Advances in analytical chemistry techniques are critical for both fundamental research and industrial applications. Catalytic nitrogen fixation offers an energy‐efficient alternative to the Haber–Bosch process, enabling ammonia production under mild conditions. Robust data integrity (DI) and regulatory compliance are essential for spectroscopic measurements in pharmaceutical and contamination laboratories. Derivative spectral analysis enhances resolution and quantitation, while FTIR methods monitor lubricant oil degradation and surface films in semiconductor manufacturing. Integrated EDX–FTIR software simplifies contaminant identification, and high-performance analytical balances improve laboratory throughput and accuracy.

Objectives and overview of the study/article

• Present new iron and cobalt base‐metal complexes that catalyze nitrogen fixation to ammonia, hydrazine, and silylamine under mild conditions.
• Demonstrate a LabSolutions/AIMsolution DI-compliant infrared microscopy workflow for pharmaceutical and contaminant analysis.
• Describe the theory and applications of first to fourth derivative spectra for peak deconvolution, baseline correction, and quantitation.
• Recommend FTIR transmission methods to evaluate lubricant oil degradation according to ASTM E2412.
• Introduce EDXIR-Analysis software for integrated elemental and molecular identification of contaminants.
• Highlight features of Shimadzu’s AP W-AD UniBloc analytical balances for rapid, stable weighing.

Methods and instrumentation

• Catalytic nitrogen fixation: iron(I) and cobalt(I) dinitrogen complexes with PCP-type pincer ligands; reductants (KC8), proton sources, silylating agents; IR monitoring of N≡N stretching by FTIR.
• Regulatory compliance: AIM-9000 IR microscope controlled by AIMsolution software linked to LabSolutions IR and LabSolutions DB/CS for audit trails, user management, and secure report sets.
• Derivative spectra: Savitzky–Golay smoothing and differentiation in LabSolutions IR to obtain first through fourth derivative spectra.
• Oil degradation: transmission FTIR with Specac Pearl horizontal liquid cell to detect water contamination, oxidation/nitration bands.
• EDX–FTIR integration: EDX-7200 energy dispersive X-ray spectrometer and IRXross FTIR interfaced via EDXIR-Analysis software.
• Analytical balances: AP W-AD Series UniBloc design for fast stabilization and automatic draft-shield door operation.

Main results and discussion

• Iron catalyst achieved 252 equiv. NH3 and 68 equiv. N2H4 per catalyst at –78 °C; anionic Fe(0)–N2 intermediate identified by IR and X-ray.
• Cobalt complexes delivered up to 371 equiv. N(SiMe3)3 per catalyst; electronic substituents modulate π back-donation and activity.
• AIMsolution DB/CS workflow met DI requirements, automating measurement control, data storage, audit logs, and electronic report approval.
• Derivative spectra separated overlapping peaks, confirmed broad and shoulder bands in UV-aged PET, protein secondary structure, and SiO2 film quantitation by PLS (r2 improved from 0.9769 to 0.9908 after second derivative).
• FTIR transmission detected lubricant oil oxidation and nitration, enabling condition-based maintenance.
• EDXIR-Analysis streamlined contaminant fingerprinting by combining elemental maps and IR spectra.
• AP W-AD balances demonstrated rapid response, stable readings, and ease of use through automatic doors.

Benefits and practical applications

• Base-metal catalysts reduce energy and carbon footprint for ammonia and silylamine production.
• DI-compliant IR microscopy ensures reliable contaminant and QC analysis in regulated environments.
• Derivative processing enhances spectral interpretation in materials research, polymer aging, and protein studies.
• FTIR‐based lubricant monitoring extends equipment life and prevents failure.
• Integrated EDX–FTIR analysis accelerates forensic, failure analysis, and quality investigations.
• High‐performance balances improve throughput in chemical, pharmaceutical, and industrial labs.

Future trends and applications

The drive toward greener ammonia synthesis will focus on electrochemical and photo-driven processes using earth-abundant metals. DI-compliant software will expand to other spectroscopic modalities and cloud-based platforms. Advanced chemometric and machine-learning techniques will leverage derivative spectra for automated component analysis. FTIR monitoring of lubricants and surface films will integrate with IoT sensors for real-time condition monitoring. Multimodal analysis combining EDX, FTIR, Raman, and mass spectrometry will become standard in contamination and forensic laboratories. Analytical balances will further enhance connectivity and automated workflows.

Conclusion

This collection of studies and applications underscores significant methodological advances in analytical chemistry. From sustainable nitrogen fixation catalysts to robust DI-compliant IR workflows, enhanced spectral processing, integrated elemental–molecular analyses, and improved weighing technologies, these innovations address critical needs in research, industrial quality control, environmental monitoring, and regulatory compliance.

References

[1] D. V. Yandulov, R. R. Schrock, Science 2003, 301, 76–78.
[2] Y. Tanabe, Y. Nishibayashi, Chem. Soc. Rev. 2021, 50, 5201–5242.
[3] K. Arashiba, Y. Miyake, Y. Nishibayashi, Nat. Chem. 2011, 3, 120–125.
[4] Y. Ashida et al., Nature 2019, 568, 536–540.
[5] Y. Ashida, Y. Nishibayashi, Chem. Commun. 2021, 57, 1176–1189.
[6] S. Kuriyama et al., Bull. Chem. Soc. Jpn. 2022, 95, 683–692.
[7] S. Kuriyama et al., Inorg. Chem. 2022, 61, 5190–5195.
[8] Y. Tanabe, Y. Nishibayashi, Coord. Chem. Rev. 2019, 389, 73–93.
[9] A. Savitzky, M. J. E. Golay, Anal. Chem. 1964, 36(8), 1627–1639.
[10] ASTM E2412-19, Standard Practice for Evaluating Used Lubricating Oils by Fourier Transform Infrared (FT-IR) Spectrometry.