REACT - Instrumentation
REACT core facility provides a range of instrumentation and services for catalysis research. All instrumentation and services are available to Northwestern students, students of outside universities, and industrial researchers.
A current list of REACT's instrumentation and services rates is available here.
If you have any questions or comments about the core’s capabilities, are interested in using the lab's equipment, or would like more details about rates, please contact REACT Operations Director Neil Schweitzer for more information.
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- Gas/ Vapor Phase Reactions
- Liquid Phase/ High Pressure Reactions
- High-Throughput Photocatalysis
- SURFACE AREA/ PORE STRUCTURE ANALYSIS
- Modular GC/ MS Gas System
- CO2/H2O Breakthrough System
- Spectroscopy Lab
- Temperature Programmed Experiments/ Chemisorption
- in situ Infrared Spectroscopy
- Mass Spectrometry
- Breakthrough/Permeability Testing Station
- UV/ Vis Raman In Situ
- Atomic Layer Lab
Gas/ Vapor Phase Reactions
REACT houses a modified BenchCAT 4000 reactor system from Altamira Instruments. The BenchCAT consists of four, fully automated, independently operated, plug-flow reactors used for catalyst screening and kinetic studies. Each station utilizes three to five mass flow controllers, a high temperature furnace (maximum temperature of 1100°C), a temperature controlled vapor generator, gas pressure safety equipment, and is equipped with an on-stream gas chromatography system (GC) for direct measurement of reaction products. Users may customize the station to test user-defined chemistries or use standardized protocols and established chemistries to compare their materials to benchmark material data provided by REACT. Standard chemistry and station configurations are described below:
STATION 1
Station one is primarily used for oxidative gas phase chemistry. Specific protocols have been set for the oxidative dehydrogenation of propane. It is equipped with three mass flow controllers and an Agilent 7890A GC system utilizing an FID and an Activated Research Company Jetanizer, which allows the FID to analyze CO and CO2 in addition to hydrocarbon products.
STATION 2
Station two is primarily used for non-oxidative gas phase chemistry. Specific protocols have been established for 1-butene isomerization. It is equipped with three mass flow controllers and an Agilent 6850 GC system utilizing an FID detector (for hydrocarbon analysis only).
STATION 3
Station three is primarily used for oxidative, vapor-phase chemistry. Specific protocols have been established for ethanol oxidation and carbon monoxide oxidation. It is equipped with three flowmeters, a temperature controlled bubbler system for vapor generation, and an Agilent 7890A GC system utilizing an FID and an Activated Research Company Jetanizer.
STATION 4
Station four is primarily used for non-oxidative gas or vapor phase chemistry. Specific protocols have been established for ethylene hydrogenation. It is equipped with five flowmeters, a temperature controlled bubbler system for vapor generation, and an Agilent 7890A GC system utilizing an FID.
The core provides inert gases for each station, reagent gases for standardized protocols, operating gases for all the GC’s, and reactor consumables. Customers are responsible for providing specialty gases and liquids.
Liquid Phase/ High Pressure Reactions
REACT houses three 4590 micro bench top autoclave Parr reactors. The Synthesis Parr Reactor is intended for high pressure, liquid phase catalyst testing and is rated up to 350°C and 200 bar. The reactor is accompanied by a 4848 control box that is used to control the reactor temperature, control the magnetic stirrer speed, and precisely measure the pressure. Additionally, the reactor is accompanied by a custom built, gas manifold system, which allows the introduction of three separate gases. The headspace gas can be sampled and analyzed on the GC.
The Gas Sampling Parr Reactor is similar to the Synthesis Reactor but with mass flow controllers to continuously add reactant gas, and the ability to continuously sample the output product gas with GC.
The Liquid Sampling Parr Reactor is similar to the Synthesis Reactor with a 4878 Automated Liquid Sampler attached to sample small aliquots of liquid reactant mixture during a reaction run
The HPLC Reactor is a custom designed and constructed liquid phase batch reactor. The system consists of a Parr reactor vessel equipped with a circulating pump and a series of valves used to inject small aliquots of the reactive solution directly into an Agilent 1200 HPLC system, providing direct measurements of reactant and product concentrations as a function of time during the reaction. The entire system is contained within a flammable atmosphere rated convection oven and is rated to 80 °C. Using a custom built gas manifold system, the Parr vessel can be pressurized with reactive and unreactive gas to 5 bar. The system is monitored and controlled using a custom built LabVIEW module and can accommodate either liquid or powder catalysts.
High-Throughput Photocatalysis
The core has a custom designed and constructed 16-well photoreactor, based off the design by the Castellano lab at North Carolina State University (see https://doi.org/10.1063/1.4915349). This reactor consists of a temperature-controlled shaker plate with independently-controllable LEDs at the bottom of each well. Vials of reactant are placed in each well and can be purged and backfilled with a gas mixture of the users’ choice, or left under vacuum. Pressure transducer caps are fitted to each vial to allow continuous monitoring of headspace pressure, and the headspace gas can be sampled at intervals and analyzed using the attached GC.
Surface Area/ Pore Structure Analysis
The Micromeritics 3Flex is the state-of-the-art instrument for measuring surface area and pore characteristics of solid powders. Fully automated, this instrument measures data on three separate samples simultaneously with minimal user labor required. Furthermore, its advanced vacuum system is ultra-stable allowing enhanced resolution for low-pressure measurements (i.e. higher accuracy for low surface area materials and small pore sizes!). REACT has established protocols for measuring nitrogen, krypton, and carbon dioxide isotherms. However, there is virtually no limit to the nature of the adsorbate as user-supplied gases and vapors can be accommodated. For these measurements, a Micromeritics Iso-controller precisely controls the sample temperature between 0°C and 80°C.
Modular GC/MS Gas System
The modular GC/MS Gas system is a closed loop gas system with a metal bellows circulation pump. It can be used to circulate up to three different reactant gases or gas mixtures through any user-supplied reactor (thermal, photoreactor, or electrochemical reactors are all possible). The gas composition is continuously monitored using a GC/MS system. The low volume of the gas loop makes this system ideal for isotopic labeling studies, where small volumes allow expensive isotopically labeled gases to be conserved. CO2/H2O Breakthrough System
The CO2/H2O Breakthrough system is a similar system to the modular GC/MS system, but using a LI-COR LI850 IR detector to monitor CO2 and H2O concentrations in the gas loop. It can also be run in an open-loop configuration if desired. The system includes a water bubbler for humidity control. An ideal use for this system would be to measure CO2 uptake values for direct air capture CO2 capture materials.
CO2/H2O Breakthrough System
The CO2/H2O Breakthrough system is a similar system to the modular GC/MS system, but using a LI-COR LI850 IR detector to monitor CO2 and H2O concentrations in the gas loop. It can also be run in an open-loop configuration if desired. The system includes a water bubbler for humidity control. An ideal use for this system would be to measure CO2 uptake values for direct air capture CO2 capture materials.
Spectroscopy Lab
Temperature Programmed Experiments/ Chemisorption
The AMI-200 is used for conducting temperature programed experiments and pulse chemisorption studies. These experiments allow the user to measure the active surface area of a material, characterize the red-ox properties of a surface, measure the desorption characteristics of adsorbates, and even measure single-point BET surface areas after various treatments. Gases provided by the center include H2, O2, CO, CO2, N2O and NH3. A temperature-controlled bubbler system is also available for the introduction of vapors in the 0-80°C range.
In-situ Infrared Spectroscopy
The Thermo 6700 infrared spectrometer is equipped with a Harrick Praying Mantis diffuse reflectance infrared Fourier Transform spectrometer (DRIFTS) attachment for analyzing solid powder surfaces under gas/vapor atmospheres and light illumination. Powder samples can be exposed to a wide variety of gases up to 550°C. The reaction chamber is also equipped with a quartz observation window, which can be utilized to shine lasers or broadband light sources. The system uses a custom-built gas manifold; various gases including Ar, H2, O2, CO, CO2, 13CO2, NH3, N2O, and D2 are available for users. A bubbler is also available for the introduction of vapors. Finally, a custom-designed, injection system has been installed for the dedicated introduction of pyridine vapor to the measurement chamber.
The Thermo-iS50 infrared spectrometer is uses a custom built gas manifold system designed for steady-state isotopic transient kinetic analysis (SSITKA) experiments. The system uses fast switching valves and a transmission, IR reaction chamber with low dead volume rated to 350°C. These features, with the use of our UGA-100, enable the accurate measurement of the dynamic bonding and desorption characteristics of reactive surface species. Additionally, this system is also used for gas-phase, breakthrough adsorption measurements and quantitative adsorption uptake measurements. The core provides the same gases as the Thermo 6700.
Mass Spectrometry
The Universal Gas Analyzer – 100 is a portable, mass spectrometer intended for sampling gas streams at atmospheric pressure. The detection limit is m/z=0-100 amu. This unit is intended as an add-on feature that can be used in conjunction with the other equipment available in the Core. Additionally, the unit is mobile and can be reserved for use as an add-on for equipment in your own lab. All that is required is a 1/8” Swagelok connection. Analysis software and computer are provided.
Breakthrough/Permeability Testing Station
The Breakthrough/Permeability Testing Station is designed to measure gas permeability through membrane materials and gas uptake values on absorbent materials. It can be used to test materials for gas separations or gas purification. It consists of a set of flowmeters and path switching valves to route input gases to material holders, and a SRS QMS Series universal gas analyzer for analysis of the output gas stream.
UV/Vis Raman In Situ
The UV/Vis Raman In Situ system is a purpose designed in situ Raman spectrometer intended for analyzing solid powder and film samples under reactive/inert gas and elevated temperature conditions. Two excitation wavelengths are currently available: 244 nm (deep UV) and 488 nm (blue). Reaction chamber is a fluidized bed, which is intended to minimize the unwanted laser-sample interactions as well as to improve homogenizing the sample-gas interactions. Equipped with a gas manifold and temperature controller, the powder or film samples can be exposed to a wide variety of gases up to 800°C. Gases provided by the center currently include hydrogen, oxygen, carbon dioxide, and inerts. A bubbler and a vaporization chamber are also available for the introduction of volatile and non-volatile vapors, respectively, such as water, alcohols, and hydrocarbons. Inquire about other reactive gas/vapor options.
Atomic Layer Deposition Lab
Atomic Layer Deposition
The Arradiance GEMStar-8 Thermal Atomic Layer Deposition (ALD) Benchtop System comes complete with 4 ALD precursor ports, four oxidizer/reducer ports, and an ozone generator. REACT provides precursors and standard coating recipes for alumina, silica, zirconia, and titania deposition. Users are permitted to supply alternative precursors to suit their needs. Our sample holders have been specially customized for deposition onto powders.