3 Flex: High Precision Gas Adsorption for Surface Area and Porosity Measurements

Porosity, Surface Area, Chemisorption, and Temperature Programmed Techniques

• Chemisorption and dynamic adsorption investigations to characterize active surfaces
• Precise gas adsorption for determining surface area and porosity
• Vapor sorption for studies tailored to specific applications
• Analysis sequencing for automated measurement of chemisorption, physisorption, and dynamic sorption on a single sample

Description

The 3Flex advanced adsorption analyzer is designed for the precise measurement of surface area, pore size, and pore volume in powders and particulate materials. It utilizes standard methods or user-customized protocols to characterize various materials, including catalysts, adsorbents, zeolites, metal-organic frameworks (MOFs), active pharmaceutical agents (APIs), excipients, and various porous and non-porous substances.

The 3Flex excels in gas or vapor adsorption analysis of microporous (<2 nm) and mesoporous (2 to 50 nm) materials, providing superior accuracy, resolution, and data reduction. A chemisorption option expands the application scope to encompass chemical and physical adsorption, enabling the characterization of the texture and active surface of catalysts, catalyst supports, sensors, and diverse materials.

The thermal conductivity detector (TCD) option introduces dynamic chemisorption and temperature-programmed methods and broadens the range of analytical techniques available within a single adsorption analyzer. This option adds temperature-programmed oxidation (TPO), reduction (TPR), desorption (TPD), and surface reactions (TPSR) for the measurement of textural properties and chemisorption.

For further versatility, the TCD analysis range can be extended with an option for pulse chemisorption through the incorporation of an automated injection loop. The TCD additionally includes a pulse chemisorption TCD.

Features and Benefits

High Resolution, High-Throughput Physisorption, and Chemisorption Instrument

Acknowledged as the leading instrument in material surface characterization, the 3Flex has emerged as essential tools for delivering high-resolution adsorption and desorption isotherms. It contributes to the advancement and validation of fundamental understanding, important for the development of methodologies and process improvements.

Extend and Increase Your Knowledge

With the 3Flex, users can fine-tune experimental parameters to enhance their understanding of the material. This analyzer can analyze a sample using three distinct probe gases simultaneously, each on a separate analysis port, all within a single run.

Extend Your Range of Study

Expand the resolution capabilities beyond micropores to the ultramicroporous level. The sophisticated transducer technology and vacuum control of the 3Flex enable the collection of adsorption isotherms and pore size distributions for materials featuring pores as minute as 0.3 nm.

Optimize Your Material

Employing the 3Flex provides valuable insights to validate your theories and rationalize the design and synthesis of MOFs, activated carbons, zeolites, and similar products.

Leverage the high throughput results derived from the 3-port mesopore and micropore design of the 3Flex for swift characterization and understanding of the surface area, porosity, and adsorption capacity of high-performance materials.

Specifications

Source: Micromeritics Instrument Corporation

Technology

Advancements in Performance and Technology

• Three adaptable analysis ports to cater to the specific requirements of the workflow.
• Delivers exceptional mesopore/micropore, physisorption, or chemisorption analyses.
• Provides configurable ports for krypton analysis of low surface area materials.
• Analysis sequencing of experiments enables the collection of surface area and porosity using physisorption; active area and crystallite size through chemisorption; and TPx data without removing the sample from the analyzer.
• The standard configuration includes vapor sorption capabilities, and an optional heated vapor source is available to expand the analysis range.
• The dedicated pressure transducer at the Po port enables continuous monitoring of saturation pressure.
• The ultra-clean manifold design incorporates hard-seal valves and chemically resistant metal seals, ensuring chemical compatibility, increased evacuation speed, vacuum performance, and the lowest outgassing rate in the industry.
• Isotherm data collection starts in the 10^-6 Torr range (10^-9 relative pressure range for N₂).
• Quickly collect high-resolution adsorption isotherms using advanced dosing methods, proprietary hardware, and analyzer control of pressure and volume adsorbed specifications.
• MicroActive^™ Data Reduction software offers potent yet user-friendly data analysis.
• Analyze a sample with three separate adsorbent gases concurrently, one at each port, in a single analysis.
• The compact footprint conserves valuable bench space.

Configurations

Physisorption Option
 

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High-Resolution Isotherms

The novel manifold design and integrated control system create an exceptionally stable environment for pressure and temperature measurements. Alongside hardware enhancements, multiple software improvements have been introduced, including a new advanced dosing method that enables the mixing of pressure and volume increments.

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Vapor Isotherms

A comprehensive collection of fluid properties for fixed gases and commonly employed vapors is incorporated to optimize analysis capabilities. Isotherm data can be effortlessly gathered using hydrocarbons as the adsorptive.

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The 3Flex Chemisorption Option

Catalyst Characterization: The Chemisorption Option

With the chemisorption option, the 3Flex is set up to conduct chemical adsorption analyses, providing researchers with valuable insights into the physical or chemical properties of catalysts, catalyst supports, and various other materials.

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This adaptable instrument allows users to transition from chemisorption to physisorption analysis within minutes.

• A standard high-precision mass flow controller ensures highly accurate and programmable gas control.
• VCR seals enhance system cleanliness, reduce outgassing rates, and provide low outgas rates and base pressures, resulting in precise low-pressure chemisorption isotherms and the capability to measure oxygen-sensitive materials.
• It has up to a total of sixteen gas inlets, allowing the investigation of multiple probe gases, maximizing efficiency, and expanding the range of applications.
• The high-temperature furnace, reaching up to 1100 °C, offers rapid and precise ramp rates to the desired temperature, featuring precise temperature control and repeatability (±1 °C).
• Advanced temperature control ensures accuracy and repeatability in monotonic isotherms.
• The new high-temperature, precision quartz cell enhances accuracy and sensitivity, especially for challenging analyses.
• Heated vapor can also serve as the adsorptive for chemical adsorption analyses.
• The design facilitates a swift transition from chemisorption to micropore physisorption within minutes.
• Kalrez, Vition, or Buna O-rings offer maximum flexibility for chemical compatibility.

Only optional level 2 TCD is offered.

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Advanced Hardware Flexibility: A sixteen-inlet gas manifold is standard with the chemisorption capability. For precise and repeatable sample preparation during sample activation, a mass flow controller (MFC) is employed for flow control. The MFC is included in the standard chemisorption hardware.

In situ Sample Preparation and Activation: In situ preparation and activation provide an entirely automated method, eliminating the need for user intervention. This seamlessly integrates activation and analysis into a straightforward and user-friendly application. Flexible pre-treatment options for reduction, oxidation, evacuation, and purging are available.

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Sample Analysis Options

• Gas selection
• Measurement of free space at both ambient and analysis temperatures
• Dosing capabilities from gas inlets or vapor sources
• Dosing options integrated into the pressure table, providing the ability to modify pressure increments, volume dose increments, and equilibrium interval times between data points
• Automated iteration of isotherms for analyzing reversible sorption

Chemi-TCD Option

Perform High-Resolution TPR, TPO, and TPD Experiments

Enhanced for even greater capabilities, this instrument is the industry's most esteemed choice for both physisorption and chemisorption. The inclusion of the integral thermal conductivity detector provides users with dynamic chemisorption analyses, enabling the performance of TPR, TPO), desorption TPD, and reactions TPRx.

The TCD option allows users to explore the temperature dependence of specific adsorption or desorption process profiles for catalysts and adsorbents. Additionally, it encompasses pulse chemisorption, consolidating multiple functionalities into one highly capable instrument.

Chemi-TCD Available Configurations:

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Included Features of the TCD Option:

• The newly enhanced MicroActive interactive software records time, temperature, and TCD signal. Alongside data collection, a comprehensive set of signal processing tools is available to convert raw data into sample property information.
• These tools encompass peak integration, peak deconvolution (curve fitting), and the calculation of active surface area, crystallite size, and dispersion.
• Featuring industry-exclusive localized loop valve temperature measurement and control, this enhancement improves precision, signal detectability, and repeatability in the TCD signal.
• Offering full versatility, the system allows for a seamless transition from chemisorption experiments to physisorption analysis in a matter of minutes.

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Accessories

Chiller Dewar

Liquid Recirculation System

The Micromeritics Chiller Dewar operates as a closed-loop recirculating system, employing a high surface area copper coil for efficient heat transfer between the dewar and recirculating liquids. Temperature control is achieved using an external recirculating bath or chiller bath, which are both available as accessory items.

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Source: Micromeritics Instrument Corporation

ISO Controller

Sub-Ambient, Thermoelectric Cooled Dewar

Micromeritics' ISO Controller employs thermoelectric cooling based on the Peltier principle. The unit maintains a consistent temperature between -5 °C to 80 °C for absorption analysis using CO₂, N₂, and other gases. The device achieves rapid cooling and efficient temperature maintenance with minimal electrical current consumption.

The dewar section is positioned on the instrument dewar elevator and subsequently elevated into place for analysis.

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Cryostat I

Single-Stage Cryogenic Refrigerator Based on the Gifford-McMahon Principle

The Micromeritics Cryostat I operates as a closed-cycle cryocooler, relying on the Gifford-McMahon (GM) refrigeration principle.

It utilizes helium gas obtained from a helium compressor to achieve cryogenic temperatures. It eliminates the requirement for liquid nitrogen and can reach temperatures below 77 K of liquid nitrogen.

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Source: Micromeritics Instrument Corporation

Physi–Consumables and Supplies

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Chemi–Consumables and Supplies

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TCD – Consumables and Supplies

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Application

Metal-Organic Frameworks and Porous Organic Polymers

Enabling the investigation of energy storage and gas separation with MOFs and porous organic polymers (POPs).

Investigate the Influence of Hydrogen Adsorption Enthalpy

Flex and 3Flex possess the capability to swiftly transition from physisorption to chemisorption, enabling exploration for enthalpy associated with ligand influence.

Determine the Influencing Relationship of Surface Area, Pore Volume, and Substrate/Analyte Interactions for Uptake, Capacity, and Release Evaluations

The 3Flex can analyze a sample using three distinct probe gases concurrently, each allocated to a separate analysis port, all in a single run.

Evaluate Optimal Small Pore Size as a Strategy to Enhance Hydrogen–Framework Interactions

Advanced gas management and temperature control enable precise and accurate micropore and ultra-micropore (<0.7 nm) measurements.

Advanced Pore Size Analysis with NLDFT Models

The MicroActive™ data software allows users to visually capture the desired isotherm data range through an intuitive and interactive user interface. This reduces the time and effort needed to convert data into textural information, including surface area and pore size.

The MicroActive user interface also facilitates the easy copying and pasting of data into the preferred software for additional analysis or custom plotting. The robust reporting software also offers features such as exporting data to a spreadsheet, saving to PDF, or printing reports.

Advancing the Understanding of Strategy and Synthesis in Zeolite Design

Quantitatively Determine the Number of Surface Active Sites for Catalytic Potential

Supply information regarding monolayer uptake, metal area, dispersion, and crystallite size of the catalysts. The exceptional versatility of the Flex family allows for swift transitions from physisorption analysis to chemisorption analysis within minutes, enabling comprehensive characterization within a single instrument.

Determine if Zeolite Processing has Resulted in Loss of Structure or Degradation

The sophisticated design of the Flex and 3Flex offers industry-leading micropore resolution. It also provides supplementary information to X-Ray diffraction, aiding in the resolution of minor structural defects caused by processing.

The Advanced Design of the 3Flex Provides Industry Leading Resolution and Accuracy

Acquire valuable insights into pore architecture to improve understanding of diffusion rates, transport, and selectivity.

Gain Valuable Data for Improving Activated Carbon Adsorbents and Catalyst Performance

Determine Adsorption Dynamics in Regard to Resident Time for Performance in Fixed Bed and Flow Through Systems

Collect valuable data to understand how surface area, pore volume, and pore size distribution influence performance.

Gain Valuable Insight of Structural and Chemical Heterogeneity Influence on Adsorption Dynamics

Advanced gas management, hard-seal valves, and metal seals, combined with precise temperature control, enable accurate and precise micropore measurements.

Evaluate Temperature and Chemical Deactivation Processes in Regard to Porosity and Surface Activity

Precise temperature and gas control guarantee repeatable analytical data from sample to sample, batch to batch.

High-Resolution and Vapor Isotherms

The updated manifold design and integrated control system establishes an exceptionally stable environment for pressure and temperature measurements. Beyond hardware enhancements, the software has been improved, introducing a new advanced dosing method that enables the combination of both pressure and volume increments.

The 3Flex comes equipped with a comprehensive library of fluid properties for fixed gases and commonly used vapors. Collecting isotherm data is made seamless by employing hydrocarbons as the adsorptive.

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Software

Data Reduction and Control Software

MicroActive for 3Flex – Data Reduction and Control Software

• Interaction with adsorption/desorption data is direct. Adjusting the calculation bars provides the user with instant updates on new textural properties.
• Click-and-drag bars simplify the selection of the calculation range, reducing the need for dialog boxes, and tunneling of dialogs to specify calculation parameters.
• The Report Options editor allows users to define reports with on-screen previews.
• It includes a Python programming interface for user-defined reports.
• The graphic interface enables user-selectable data ranges for direct modeling of BET, BJH, t-Plot, Langmuir, DFT interpretation, and more. The MicroActive isotherm analysis suite offers an extensive array of NLDFT models for calculating pore size distributions.
• Overlay up to 25 files, allowing for the superimposition of mercury intrusion results with pore size analysis from the 3Flex.

t-Plot analysis of N₂ at 77 K on MCM-41 silica. The t-Plot calculation shows this is not a microporous material despite the large gas capacity. Image Credit: Micromeritics Instrument Corporation

3Flex Interactive Reports Include:

• Isotherm
• Langmuir Surface Area
• BET Surface Area
• t-Plot
• Alpha-S Method
• BJH Adsorption and Desorption
• Dollimore-Heal Adsorption and Desorption
• Horvath-Kawazoe
• MP-Method
• Dubinin-Astakhov
• Dubinin-Radushkevich
• DFT Pore Size and Surface Energy
• User-Defined Reports (5)

NLDFT Dual Isotherm Deconvolution and Pore Size Distribution

The NLDFT Advanced PSD, utilizing Dual DFT modeling, enables users to merge data from nitrogen/argon and carbon dioxide isotherms. This comprehensive approach provides a complete pore size distribution for materials, especially those like carbon slit pores, where molecular-sized pores are present.

This method extends the range of pore size analysis to smaller sizes compared to standard nitrogen analysis. This is because CO₂ can access ultra-micropores that N₂ cannot reach at cryogenic temperatures due to diffusion limitations.

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This advanced NLDFT method enables the determination of the pore size distribution of a sample utilizing two isotherms. In this instance, CO₂ adsorption (depicted in green) at 77 K and N₂ (shown in red) are employed to compute a unified pore-size distribution. There is no need to manually integrate distributions from CO₂ and nitrogen—instead, a single distribution is derived using both isotherms.

Mercury Porosimetry/Gas Adsorption Overlay

MicroActive for the 3Flex incorporates a robust feature enabling users to overlay pore size distributions obtained from mercury porosimetry onto those derived from gas adsorption. This innovative import function facilitates the swift examination of micropore, mesopore, and macropore distributions within a single application.

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Overlay of BJH desorption and mercury intrusion log differential pore size distributions for alumina pellets.

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