ProC-1C In-situ Catalysis/Pyrolysis Mass Spectrometry Analysis System

The ProC-1C in-situ catalytic/pyrolysis mass spectrometry analysis system utilises photo-composite soft ionisation technology, enabling the analysis of all components—including hydrogen, oxygen, carbon monoxide, carbon dioxide, ozone, nitrogen oxides, sulphur-containing compounds, chlorine-containing compounds, hydrocarbons, and other substances—in heat-induced catalytic, pyrolysis and oxidation reactions. thermally induced catalytic, pyrolytic and oxidative reactions (hydrogen, oxygen, carbon monoxide, carbon dioxide, ozone, nitrogen oxides, sulphur-containing compounds, chlorine-containing compounds, hydrocarbons, polycyclic aromatic hydrocarbons, etc.) with virtually no fragmentation, thereby enabling real-time, on-line analysis of the analytes directly without the need for chromatographic separation.

In catalytic science research, understanding reaction mechanisms is of paramount importance; however, such studies are often challenging and require a combination of extensive experimental evidence and characterisation techniques. In the study of gas-solid phase catalytic reactions, the most commonly used catalyst evaluation apparatus is the fixed-bed catalytic reactor, with the reactor outlet connected to a gas chromatograph. This enables the analysis of stable reaction products, thereby facilitating the evaluation of catalyst performance. However, studying reaction products alone does not provide a comprehensive understanding of the catalytic reaction process, as many key reaction intermediates are highly unstable or extremely difficult to capture, and this information is lost in conventional product analysis. Consequently, catalytic research frequently combines techniques such as infrared, ultraviolet and nuclear magnetic resonance spectroscopy to investigate species changes during catalytic reactions, thereby gaining insight into the reactions occurring on the catalyst surface. For reactive intermediates in the gas phase, in situ mass spectrometry is currently one of the most powerful detection methods.

Applications of in situ catalytic mass spectrometry in the field of gas-solid phase catalysis

In recent years, the application of photoionisation mass spectrometry in the field of catalysis has greatly aided our understanding of the mechanisms of certain key reactions. By utilising a low-pressure catalytic reactor in conjunction with photoionisation mass spectrometry, it has been possible to detect intermediate products in the reaction of synthesis gas to form olefins, confirming that acetylacetone is a key intermediate in the synthesis of low-carbon olefins. Specifically, CO and H₂ are first activated on the surface of a metal oxide to form compounds containing CH₂, which subsequently generate acetylacetone; the acetone diffuses via the gas phase into the pores of SAPO zeolite, where it is converted into low-carbon olefins at acidic sites; this mechanistic insight has advanced catalyst design, enabling product selectivity far exceeding the limits of conventional Fischer-Tropsch synthesis (Figure 1).

Figure 1. Photoionisation mass spectrometry analysis of the synthesis gas-to-olefins reaction

In methane oxidation coupling reactions, the combination of a low-pressure reactor with photoionisation mass spectrometry enables the in situ capture and detection of reactive intermediates such as methyl radicals, peroxymethyl radicals and formaldehyde (Figure 2), thereby aiding the establishment of the gas-phase reaction mechanism for this process.

Figure 2. Photoionisation mass spectrometry analysis of the methane oxidation coupling reaction

In the methanol-to-olefins reaction, the aforementioned method enables the direct capture of the reactive intermediate formaldehyde and allows the dynamic changes in formaldehyde and other products to be observed from the induction phase to the deactivation phase (Figure 3).

Figure 3. The capture and dynamic changes of formaldehyde

Performance Specifications

• Temperature control range: 25–1400 °C

• Pressure control range: 1 Torr to 0.5 MPa

• Mass detection range: 1–500 amu

• Sensitivity: 10 ppb

• Mass spectrometry resolution: >3500@(m/z=92)

• Automated data acquisition and analysis software

Ancillary equipment

• Atmospheric pressure pyrolysis reactor (Reaction temperature: room temperature to 1200°C; Vacuum level: atmospheric pressure; Material: corundum/quartz)

• Low/high-pressure pyrolysis reactors (Operating temperature: room temperature to 1400°C; Vacuum range: 10⁻¹ Pa–0.5 MPa; Material: corundum/quartz)

Product Features

• Enables online monitoring of light-, heat- and electricity-induced catalytic vapour-phase products

• Can detect unstable intermediate products such as free radicals, formaldehyde and ketones (reactor optional)

• Fast sampling speed (on the order of seconds)

• No chromatographic separation required; no polarity discrimination

• Simultaneous monitoring of multiple reaction channels via valve switching (valve optional)

• Specialised database of catalytic and pyrolysis products

• Online monitoring of products at fixed temperatures and during programmed temperature ramping

• Can be coupled with thermogravimetric analysers and infrared spectrometers

Main accessories (optional):

• Multi-channel switching valve

• In-situ thermocatalytic reactor

• In-situ photocatalytic reactor

• Combustion reactor

• Flow-through reactor

• JSR reactor

• Gas chromatography, infrared and thermogravimetric interfaces and operating software

Application scenarios

• Pyrolysis/combustion reactions

• Photocatalytic/thermal catalytic reactions

• Low-temperature oxidation reactions

• Baking/Thermal Desorption

• Petrochemicals/Coal Chemical Industry

• Solid Waste/Biomass

• Food Processing

• Cigarettes

• Fermentation

• Environmental monitoring

Application examples

Detection of intermediates in the methane oxidation coupling (OCM) reaction

Enables in-situ capture and detection of reactive intermediates such as methyl radicals, peroxymethyl radicals and formaldehyde

Monitoring of cigarette pyrolysis products

The distribution and intensity differences of pyrolysis products at different pyrolysis temperatures can be observed (m/z=162 corresponds to nicotine)

Monitoring of catalytic pyrolysis products of polyethylene

When polyethylene is treated with HZSM-5 catalyst, a significant increase in the selectivity of certain catalytic pyrolysis products can be observed

Dynamic monitoring of methanol-to-olefins (MTH) products

The formation and conversion processes of formaldehyde (a carbon deposit intermediate) and other products on different catalysts can be observed

Monitoring of coal pyrolysis products

The formation of a large number of hydrocarbon pyrolysis products can be observed in real time

Study of the MTH reaction using mass spectrometry–infrared spectroscopy coupling

Simultaneous acquisition of spectral patterns for both gas-phase desorption products and adsorption products

Summary of use

• In the field of gas-solid phase catalytic science, reaction mechanisms have long been a focus of attention. To investigate these mechanisms, various characterisation techniques must be established to obtain experimental evidence. Gas-solid phase catalytic processes generate a large number of adsorbed species and gas-phase reaction intermediates, including even short-lived radicals. In situ catalytic UV photoionisation mass spectrometry, which has been developed in recent years, utilises molecular beam sampling and photoionisation techniques to obtain information on intermediates such as short-lived gas-phase radicals. It has played a significant role in mechanistic studies of reaction systems such as FTO, OCM and MTH, with related research findings published in journals including *Science*.

• ProC-1Cin-situ catalytic/pyrolysismass spectrometryanalysis systemnot only provides stable information on gas-phase catalytic products within seconds, but also enables the in situ capture and detection of reactive intermediates such as methyl radicals, peroxymethyl radicals and formaldehyde, which is of great significance for investigating the mechanisms of gas-solid catalytic reactions. This type of in-situ catalytic UV photoionisation mass spectrometer has a mass resolution exceeding 3,500 and a sensitivity of 10 ppb, with well-optimised parameters.

The company undertakes customised and other products

We also provide bespoke customisation services for non-standard time-of-flight mass analysers and various mass spectrometer-specific spare parts, including catalytic and high-pressure pyrolysis reactors, photoionisation sources, ionisation chambers, JSR reactors, molecular pumps, MCP microchannel plates and data acquisition cards.