Catalysts are the silent workhorses of the petrochemical industry, driving critical reactions in refining and chemical production.

But what if you could optimise these catalysts in real-time, tuning them like a high-performance engine while your plant continues to run at full capacity? This is exactly what cutting-edge analytical technologies are enabling R&D leads and researchers to achieve, allowing for revolutionary precision in catalyst monitoring and optimisation.

In this article, we’ll look at high-temperature Fourier transform infrared spectroscopy (FTIR) coupled with thermogravimetric analysis (TGA), and also introduce some other important techniques used to analyse catalysts and their reaction mechanisms.

These advancements are not just lab curiosities – they’re setting new standards for efficiency, sustainability and profitability across the global petrochemical industry, where even marginal improvements in performance can realise massive cost savings. The global catalyst market is projected to grow at a CAGR of 4.4% and reach $52.7 billion by 2027, making a focus on catalyst optimisation more crucial than ever​.1

The role of catalysts in petrochemical production

Metal oxide catalysts, especially those based on alumina and titania, are crucial in many petrochemical processes including fluid catalytic cracking (FCC) and steam reforming. Catalytic performance is directly influenced by the behaviour and coordination environment of surface hydroxyls, which impact upon reaction rates, product yields and overall energy consumption.

High-temperature FTIR and TGA: a game-changer

Recent advancements in catalyst characterisation offer previously unattainable insights into the behaviour of surface hydroxyls. High-temperature FTIR coupled with TGA is one such technology, allowing for in situ measurement of surface hydroxyl and water coverage on metal oxide catalysts.

Harrick’s High Temperature Transmission Cell is ideally suited for recording transmission FTIR spectra at elevated temperatures, and when these measurements are calibrated using TGA data for the same catalyst, surface hydroxyl and water density can then be determined using only FTIR data. This permits catalyst monitoring under real-world operating conditions, enabling unprecedented control over catalytic performance. See Application Note

Key benefits of the FTIR–TGA approach:

  1. Precision catalyst optimisation: With real-time monitoring of surface conditions, engineers can adjust catalyst formulations on the fly to maximise efficiency. This is crucial in an industry where catalyst performance directly influences profitability.
  2. Real-time feedback under harsh conditions: This technology has no problem operating in extreme environments, such as those found in FCC or steam reforming units. It can monitor catalysts at temperatures of up to 320 °C, which mirror the conditions needed for these processes.
  3. Cost savings: By optimising reactions in situ, petrochemical companies can extend catalyst life and reduce the need for expensive shutdowns. For example, a 2% efficiency improvement in FCC units, which are the backbone of most refineries, can save millions annually. These cost savings could be pivotal as refineries strive for higher margins while continuing to process heavier crudes.1

Applications in FCC and hydrogen production

Two core petrochemical processes, FCC and steam reforming, can benefit greatly from this advanced monitoring approach.

FCC

FCC is vital for the production of high-value products like petrol, diesel and feedstock olefins from heavy crude fractions. For these energy-intensive processes, even small improvements in efficiency can have large financial implications (as mentioned above). Real-time optimisation of catalyst performance can significantly lower feedstock costs while increasing product yields​.1

Steam reforming

Hydrogen production, a cornerstone of the petrochemical industry, is heavily reliant on steam reforming. As the demand for hydrogen grows,1 particularly due to low-carbon initiatives, it will be critical to improve the efficiency of this process. Steam reforming uses nickel-based catalysts that are prone to degradation due to carbon buildup, but by leveraging FTIR–TGA, operators can monitor surface carbon levels and adjust conditions to mitigate fouling and extend catalyst life.

Sustainability and environmental compliance

Efficient catalysis is ever more vital in an industry under pressure to reduce its carbon footprint. Adopting real-time monitoring to optimise catalyst performance can reduce CO2 emissions by 5–10%, helping companies align with global sustainability goals.

According to the International Energy Agency (IEA), this could play a key role in achieving emissions reduction targets across refining sectors and contribute to a more sustainable petrochemical industry​,1 as well as improving overall process efficiency and supporting regulatory compliance.

A notable recent study used in situ monitoring to characterise more sustainable ceria-based catalysts for the synthesis of dimethyl carbonate from CO2 and methanol.2 Specifically, ceria nanorod catalysts are normally produced under energy-intensive hydrothermal conditions (i.e., at high temperature and pressure) for extended periods. The researchers found that nanorods prepared in just 30 minutes at reflux showed superior catalysis of dimethyl carbonate production, employing Harrick’s High Temperature Cell to demonstrate higher CO2 adsorption by these catalysts.

Therefore, integration of in situ catalyst monitoring technologies offers a clear route to balancing profitability with sustainability – a critical concern as governments around the world push for more aggressive climate action.

Combining other techniques for catalyst studies

Raman and DRIFTS

Collaborators from the Shanghai Institute of Technology and University of Idaho combined Raman spectroscopy and diffuse reflection infrared Fourier transform spectroscopy (DRIFTS) to explore how methanol reacts on copper oxide-based catalysts, which are potentially important for methanol steam reforming. The study used Harrick’s Praying Mantis™ High Temperature Reaction Chamber and Diffuse Reflection Accessory to observe changes in the catalysts and reaction products at different temperatures. It was possible to follow changes in catalyst composition and identify formation of products like formaldehyde and CO2, distinguishing between the vapour phase and surface-bound states. Insights from such studies can help extend the use of methanol, which can be derived from renewable resources, to support the transition to greener energy systems. Read the full Application Note

SEM, EDS, FTIR, XPS and others

Other researchers used a mix of lab techniques to investigate some transition metal carbides (VC, NbC and TaC) as affordable materials for capturing and converting CO₂. They employed scanning electron microscopy (SEM) for structural analysis, energy dispersive X-ray spectroscopy (EDS) for elemental analysis, FTIR for chemical characterisation and X-ray photoelectron spectroscopy (XPS) for surface elemental composition analysis. Using Harrick’s Praying Mantis™ High Temperature Reaction Chamber, they collected DRIFTS spectra to understand how the carbide samples interacted with CO₂ and found stronger adsorption on NbC and TaC. Their results point to surface-modified transition metal carbides as promising materials for reducing CO₂.3

XAS-Raman operando analysis

A French group conducted an operando (i.e., real-time in situ) study that coupled X-ray absorption spectroscopy (XAS) with Raman spectroscopy to analyse titania-supported oxomolybdate catalysts during methanol oxidation. Reactions were conducted in Harrick’s Raman High Temperature Reaction Chamber. This approach enabled them to observe rapid structural changes in the catalyst under working conditions, with partial reduction of molybdenum sites under methanol flow. These results highlight the value of combined spectroscopic techniques in gaining insight into catalytic processes, and should pave the way for structure–reactivity relationship studies to better understand the catalytic mechanisms. Learn more

PM-IRRAS, OES and mass spectrometry

Non-thermal plasmas are partially ionised gases generated by exposure to electric fields, and may be integrated with conventional catalysis to develop new chemical processes. In a recent study, US-based researchers applied polarisation modulation infrared reflection-absorption spectroscopy (PM-IRRAS), together with optical emission spectroscopy (OES) and mass spectrometry, to investigate the deposition and activation of carbonaceous species when methane was passed over various surfaces under an argon plasma jet.

The PM-IRRAS technique uses a grazing-angle configuration to ensure the IR beam reflects off the sample surface, thereby permitting characterisation of surface-bound species. By combining PM-IRRAS measurements from the Harrick RefractorReactor™  with other spectroscopic data, the study identified production of C2 and C3 hydrocarbons in a two-step process of plasma-stimulated deposition and activation, with different chemistries observed for nickel, silica and KBr surfaces. This multimodal analytical setup may find future application in plasma-enhanced catalysis.4

The future of catalyst technology in petrochemicals

The need for innovation in catalyst technology will only increase with the projected growth of the global petrochemical industry over the next decade. Combining FTIR with other analytical techniques offers ample opportunity to understand and optimise performance, enabling engineers to extend the operational lifespan of catalysts and maximise process efficiency under real-world conditions.

The economic benefits are clear: reduced operating costs, fewer shutdowns and more efficient resource use. But beyond that, the ability to fine-tune reactions in real time opens up new possibilities to improve sustainability and adapt to changing regulatory demands in an increasingly competitive global market.

As the industry evolves, those who leverage advanced catalyst monitoring and optimisation technologies will lead the way in process efficiency, profitability and reduced environmental impact. This isn’t just the future of catalysis – it’s happening right now.

 Learn more about our range of tools for catalyst research and development.

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References

1. M. Usman, A. Rehman, F. Saleem, A. Abbas, V. C. Eze and A. Harvey, RSC Adv., 2023, 13, 22717–22743.

2. W.-F. Kuan, W.-Y. Yu, F.-Y. Tu, C.-H. Chung, Y.-C. Chang, M. M. Lin, T.-H. Yu and L.-J. Chen, Chem. Eng. J., 2022, 430, 132941.

3. H. Prats, A. Pajares, F. Viñes, P. R. de la Piscina, R. Sayós, N. Homs and F. Illas, ACS Appl. Mater. Interfaces, 2024, 16, 28505–28516.

4. G. Lee, D. B. Go and C. P. O’Brien, ACS Appl. Mater. Interfaces, 2021, 13, 56242–56253.

Related resources

  1. Characterization of Surface Hydroxyls on Metal-Oxide Catalysts Using High Temperature Transmission FTIR Coupled with Thermogravimetric Analysis
  2. In Situ Investigation of Catalytic Reactions on CuO-Based Catalysts by Raman and Diffuse Reflection Infrared Spectroscopy
  3. Coupled XAS-Raman Operando Analysis of TiO2 Supported Oxomolybdate Catalysts in Methanol Conversion

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