3Flex-Surface Characterization Analyzer

• High-precision gas adsorption for measuring porosity and surface area.
• Vapor sorption for application-specific investigations.
• Chemisorption and dynamic studies for the characterization of active surfaces.
• Analysis sequencing for automated measurement of chemisorption, dynamic sorption, and physisorption on a single sample.

Powders and particulate materials can have their surface area, pore size, and pore volume measured using the 3Flex high-performance adsorption analyzer. User-customized procedures or standard techniques can be employed to characterize adsorbents, catalysts, zeolites, metal-organic frameworks (MOFs), active pharmaceutical ingredients (APIs), excipients, and a wide range of porous and non-porous materials.

The 3Flex offers exceptional accuracy, resolution, and data reduction and is well suited for gas or vapor adsorption investigation of microporous (<2 nm) and mesoporous (2 to 50 nm) materials.

3Flex can now be utilized for physical and chemical adsorption to characterize the active surface and texture of catalysts, catalyst supports, sensors, and a wide range of other materials. This is made possible by the addition of a chemisorption option.

The TCD option adds temperature-programmed and dynamic chemisorption methods, expanding the range of analytical techniques that can be performed with a single adsorption analyzer.

For evaluating textural characteristics and chemisorption, the TCD option includes temperature-programmed reduction (TPR), oxidation (TPO), desorption (TPD), and surface reactions (TPSR). With the inclusion of an automated injection loop, the TCD analytical range can be expanded with the option for pulse chemisorption. A pulse chemisorption TCD is also included in the TCD.

Features and Benefits

High Resolution, High Throughput Physisorption, and Chemisorption Instrument

The 3Flex is recognized as the most advanced material surface characterization instrument in the field. They have become critical tools for advancing and validating fundamental understanding into the creation of techniques and process improvements by offering high-resolution adsorption and desorption isotherms.

Extend and Increase Knowledge

Users can optimize experimental parameters in 3Flex to acquire a better knowledge of the material. Within a single run, the 3Flex can examine a sample with three different probe gases at the same time, one on each analysis port.

Extend the Range of Study

Extend the resolution range beyond micropores to the ultramicroporous level. Users can collect adsorption isotherms and pore size distributions for materials with pores as tiny as 0.3 nm using 3Flex’s sophisticated transducer technology and vacuum management.

Optimize the Material

Users receive useful information using the 3Flex to confirm their hypotheses and rationalize the design and synthesis of MOFs, zeolites, activated carbons, and other products. Use the high throughput findings of the 3Flex’s 3-port mesopore & micropore design to swiftly understand and characterize the surface area, porosity, and adsorption capacity of high-performance materials.

Specifications

Source: Micromeritics Instrument Corporation

Technology

Advancements in Performance and Technology

• Superior mesopore/micropore, physisorption, and chemisorption studies are available. Ports can be set up to analyze krypton in low surface area materials.
• Three customizable analysis ports adapt to the user's workflow requirements.
• The standard setup provides vapor sorption capabilities, and a heated vapor source is offered as an option to increase the analytical range.
• Analysis sequencing of experiments offers the ability to gather surface area and porosity using physisorption, active area, and crystallite size using chemisorption, and TPx data without removing the sample from the analyzer. 
• Hard-seal valves and chemically resistant metal seals are elements of the ultra-clean manifold design, which offers chemical compatibility, higher evacuation, and vacuum performance, and the lowest outgassing rate in the sector.
• Saturation pressure can be continuously monitored using a Po port equipped with a specialized pressure transducer.
• The range in which isotherm data collection starts is 10^-6 Torr (10^-9 relative pressure range for N₂).
• The MicroActive™ Data Reduction offers potent yet user-friendly data analysis.
• Gather high-resolution adsorption isotherms quickly using cutting-edge dosing techniques, exclusive hardware, and analyzer control of the adsorbed pressure and volume parameters.
• Minimal footprint preserves important bench space.
• Examine a sample concurrently using three different adsorbent gases, one for each port in a single analysis.

Configurations

Physisorption Option

Advancements in Performance:

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High-Resolution Isotherms

The novel manifold design and inbuilt control create an ultra-stable environment for pressure and temperature monitoring. Aside from hardware upgrades, there have been various software advancements, including a new sophisticated dosing mechanism that allows users to mix pressure and volume increments.

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Vapor Isotherms

To optimize analytical capabilities, a wide library of fluid characteristics of fixed gases and regularly used vapors is offered. Isotherm data can be easily acquired when hydrocarbons are used as the adsorptive.

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The 3Flex Chemisorption Option

Catalyst Characterization: The Chemisorption Option

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The 3Flex is set up to conduct chemical adsorption investigations with the chemisorption option, allowing the researcher to get important data regarding the chemical or physical characteristics of catalysts, catalyst supports, and a range of other materials.

• VCR seals ensure better system cleanliness, lower outgas rates, and lower base pressures. As a result, precise low-pressure chemisorption isotherms are obtained, as well as the capacity to test oxygen-sensitive materials.
• A standard high-precision mass flow controller allows for exceptionally accurate and customizable gas control.
• A high-temperature furnace (up to 1100 °C) offers rapid and precise ramp rates to the required temperature with accurate temperature control and repeatability (±1 °C).
• Multiple probe gases can be explored using up to sixteen gas inlets, enhancing efficiency and application range.
• Superior temperature control maintains repeatability and accuracy in monotonic isotherms. 
• The flexible design allows for a quick shift from chemisorption to micropore physisorption within minutes.
• A new high-temperature precision quartz cell boosts accuracy and sensitivity for difficult analyses.
• In chemical adsorption analysis, heated vapor can also be utilized as an adsorptive.
• Chemical compatibility is maximized using Kalrez, Vition, or Buna O-rings.

Only optional level 2 TCD is offered.

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Superior Hardware Versatility: Up to sixteen inlets are standard with the chemisorption capability. A mass flow controller (MFC) is used for flow control during sample activation to ensure accurate and consistent sample preparation. The usual chemisorption gear comes with the MFC.

In situ Sample Preparation and Activation: In situ preparation and activation offer a completely automated approach that combines analysis and activation into a single, user-friendly program, eliminating the need for human interaction. Different options for pre-treatment enable oxidation, reduction, evacuation, and purging.

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Sample Analysis Options

• Dosing from gas inlets or vapor sources.
• Automatically repeat isotherm to analyze reversible sorption.
• Gas selection.
• Free space measured at both ambient and analysis temperature.
• The pressure table has dosing options that allow users to adjust the volume dosage increment, pressure increment, and equilibrium gap time between data points.

Chemi-TCD Option

Perform High-Resolution TPR, TPO, and TPD Experiments

The most well-known and favored equipment in the industry for physisorption and chemisorption has been enhanced in strength.

TPR, TPO, TPD, and TPRx can now be carried out by the user through dynamic chemisorption analyses, thanks to the inclusion of an inbuilt thermal conductivity detector.

With the TCD option, users can utilize this extremely powerful instrument to study the temperature dependency of certain adsorption or desorption process profiles for catalysts and adsorbents, as well as pulse chemisorption.

Chemi-TCD Available Configurations: Source: Micromeritics Instrument Corporation

Included Features of the TCD Option:

• The recently updated MicroActive interactive software records the temperature, time, and TCD signal. A complete set of signal processing tools is offered in addition to data collection to convert unprocessed data into sample property information. Peak integration, peak deconvolution (curve fitting), and the computation of active surface area, crystallite size, and dispersion are examples of these tools. 
• Precision, detectability, and repeatability of the TCD signal are all improved by industry-exclusive localized loop valve temperature measurement and control. 
• Complete flexibility: in only a few minutes, go from chemisorption tests to physisorption analysis.

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Accessories

Chiller Dewar

Liquid Recirculation System

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The Chiller Dewar from Micromeritics is a closed-loop recirculating system that offers superior heat transmission between the recirculating liquids and the dewar by using a large surface area copper coil. An external recirculating bath or chiller bath, which are available as additional products, enables temperature control.

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ISO Controller

Sub-Ambient, Thermoelectric Cooled Dewar

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The ISO Controller from Micromeritics uses Peltier-based thermoelectric cooling. The unit is made to have a steady temperature, between -5 °C and 80 °C, when employing CO₂, N₂, and other gases for adsorption analysis. The device uses extremely little electrical current to quickly cool and effectively maintain temperature.

The dewar section is positioned on the instrument dewar elevator and then lifted into place for analysis.

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Cryostat I

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

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Based on the Gifford-McMahon (GM) refrigeration concept, the Micromeritics Cryostat I is a closed-cycle cryocooler. It creates cryogenic temperatures using helium gas from a helium compressor.

Liquid nitrogen is not necessary with Cryostat I, which can achieve temperatures lower than 77 K of liquid nitrogen.

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Physi–Consumables and Supplies

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3Flex Chemi-Consumables & Supplies

Chemi–Consumables & Supplies

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TCD–Consumables and Supplies

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Application

Metal-Organic Frameworks and Porous Organic Polymers

Empowering the Study of Energy Storage and Gas Separations by MOFs and porous-organic polymers (POPs).

Investigate the Influence of Hydrogen Adsorption Enthalpy

3Flex can quickly transition from physisorption to chemisorption, allowing for the examination of enthalpy related to ligand impact.

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

In a single run, the 3Flex can examine a sample with three different probe gases at once, one on each analysis port.

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

Accurate and precise micropore and ultra-micropore (<0.7 nm) measurements are made possible by superior gas management and temperature control.

Advanced Pore Size Analysis with NLDFT Models

Using an intuitive user interface, MicroActive™ Data Software enables users to graphically record the relevant range of isotherm data, saving you time and effort when converting data into textural information like surface area and pore size.

The potent reporting software allows users to export the data to a spreadsheet, save it to PDF, or print reports. The MicroActive user interface lets users copy and paste data to the preferred program for additional analysis or custom plotting.

Advancing the Understanding for Strategy and Synthesis in Zeolite Design

Quantitatively Determine the Number of Surface Active Sites for Catalytic Potential

Provide information on the catalysts’ dispersion, metal area, monolayer uptake, and crystallite size. The 3Flex's exceptional versatility enables complete characterization with a single instrument by enabling users to switch in minutes from physisorption analysis to chemisorption analysis.

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

The 3Flex’s sophisticated architecture offers the best micropore resolution in the market. It also offers complementary information and X-Ray diffraction to address small structural flaws brought on by processing.

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

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

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

Understand how surface area, pore volume, and pore size distribution affect performance.

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

Superior gas management, hard seal valves, metal seals, and precise temperature control allow for accurate and exact micropore measurements.

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

Temperature and gas control accuracy provide consistent analytical results from sample to sample and batch to batch.

High-Resolution and Vapor Isotherms

Image Credit: Micromeritics Instrument Corporation

The innovative manifold design, together with inbuilt control, creates an ultra-stable environment for pressure and temperature monitoring. Aside from hardware enhancements, software advancements include a new enhanced dosing approach that enables users to mix pressure and volume increments.

The 3Flex comes with a large library of fluid characteristics for fixed gases and regularly used vapors. Isotherm data can be easily acquired when hydrocarbons are used as the adsorptive.

Software

Data Reduction and Control Software

MicroActive for 3Flex – Data Reduction and Control Software

• Direct interaction with adsorption/desorption data is possible. The user is immediately updated with new textural properties by simply adjusting the calculation bars.
• Click-and-drag bars slide to pick the computation range, reducing the utilization of dialog boxes and tunneling of dialogs to define the calculation parameters. 
• User-customizable data ranges through the graphic interface, enabling direct modeling for BET, BJH, t-Plot, Langmuir, DFT interpretation, and more. MicroActive isotherm analysis software includes a large number of NLDFT models for estimating pore size distributions.
• Users can define reports with on-screen previews using the Report Options editor.
• Python programming interface for user-defined reports is included.
• Mercury intrusion findings can be superimposed with pore size analysis from the 3Flex on up to 25 files.

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:

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

NLDFT Dual Isotherm Deconvolution and Pore Size Distribution

The NLDFT Advanced PSD, Dual DFT modeling enables the user to use the information acquired from nitrogen/argon and CO₂ isotherms to produce a comprehensive pore size distribution on materials (such as carbon slit pores) where molecular-sized pores are present. 

When compared to traditional nitrogen analysis, the range of pore size analysis in this approach is extended to lower pore sizes. This is because CO₂ can access ultra-micropores that N₂ cannot access at cryogenic temperatures due to diffusion limitations.

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Using two isotherms, this sophisticated NLDFT approach allows you to calculate the pore size distribution of your sample. In this example, CO₂ adsorption (green) at 77 K and N₂ (red) are utilized to generate a single pore-size distribution. Users do not have to copy and paste CO₂ and nitrogen distributions since both isotherms are used to generate a single distribution.

Mercury Porosimetry/Gas Adsorption Overlay

MicroActive for the 3Flex offers a useful application that allows users to overlay pore size distributions from mercury porosimetry with gas adsorption distributions. With this new import feature, users can quickly see micropore, mesopore, and macropore distributions in a single application.

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Overlay of the different pore size distributions for BJH desorption and mercury intrusion logs for alumina pellets.

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