Micromeritics BreakThrough Analyzer

Compact, versatile, high-performance selective adsorption

Superior design minimizes dead volume & delivers accurate, experimental results
Configurable with up to 6 precision mass flow controllers and 2 vapor sources
Patented high-performance blending valves
Sample activation up to 1050 ℃
Thermostated environmental chamber provides uniform temperature control, even when using vapors
Easily connects to commercial Mass Spectrometer & Fourier Transform Infrared Analyzer (FTIR)
Secure door lock system for enhanced operator safety

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Overview

The Micromeritics BreakThrough Analyzer is a flexible gas delivery and management system for the precise characterization of adsorbent performance under process-relevant conditions. It delivers reliable adsorption data for gas/vapor mixtures using a flow-through system.

A safe and highly optimized device for collecting both transient and equilibrium adsorption data for multi-component systems. The BreakThrough Analyzer can be configured with up to six precision mass flow controllers and patented high-performance blending valves, delivering unparalleled flexibility in experimental design. The superior gas-delivery design ensures the precise control of both composition and flow rate, while minimizing dead volume.

The high-quality, stainless-steel column can hold 0.05 to 2.5 grams of adsorbent. Automated sample activation up to 1050 °C is possible with the precise, rugged, and reliable resistance furnace.

Operating pressures are controlled from atmospheric to 30 bar via a servo-positioned controlled valve. The thermostated environmental chamber delivers uniform temperature control of the entire system up to 200 °C, eliminating cold spots. The BreakThrough Analyzer secure door lock system ensures operator safety throughout the analysis.

Vapor generators can be added to the BreakThrough Analyzer to enable the use of important probe molecules such as water for experimental studies. The BreakThrough Analyzer easily connects to commercially available Fourier Transform Infrared and Mass Spectrometer systems for gas identification and quantification.

Thermostated environmental chamber prevents condensation of vapor streams
Fully automated experimental design allows for easy experimental setup
Touch screen allows for easy instrument operation and monitoring of experimental conditions
Proprietary blending valves provide remarkable advantages for gas mixing and minimization of system dead volume
Up to 6 gas inlets and 2 vapor sources offer a wide range of analysis options with exceptional flow control and blending of multiple gases
Automatic door lock ensures temperature stability during analysis and user safety
Addition of detectors and other optional accessories: system scalability enables the expasion of capabilities over time through addition of detectors and other optional accessories (e.g. mass spectrometer, GC/MS, additional vapor sources, vacuum activation, others available upon request)
Column furnace: rugged, resistance furnace with high temperature capabilities up to 1050 °C
Electropolished 316 SS sample column with a capacity of up to 2.5g and is suitable for use with powders, other diameters are available for pellets or extrudates

Breakthrough adsorption dynamic analysis

Breakthrough analysis is a powerful technique for determining the adsorption capacity of an adsorbent under flow conditions. Dynamic breakthrough adsorption provides many advantages over static adsorption measurements.

Easily collect multicomponent adsorption data
Determine adsorbate selectivity
Replicate process conditions

When conducting breakthrough analysis, sample preparation is a critical step in the analysis process to prevent pressure drop and mass transfer limitations.

Pressure drop occurs when the interstitial space between particles is too small to accommodate the flow rate of gas.
Mass transfer limitations occur when the pore size of the material is similar to the kinetic diameter of the adsorbate.

Appropriately sizing particles is therefore critical to obtain the best results.

Examining a breakthrough curve

Complete adsorption
The adsorbent completely adsorbs the adsorbate gas such that none can be detected at the outlet of the breakthrough column
Breakthrough
The adsorbate gas is first detected at the outlet of the breakthrough column. Gas continues to adsorb; however, the adsorbent is no longer able to adsorb the entirety of the gas that is entering the breakthrough column
Saturation
The adsorbent has reached saturation and can no longer adsorb the adsorbate gas, allowing it to pass through the column freely

Carbon dioxide adsorption

Single-component carbon dioxide breakthrough adsorption experiments were conducted on zeolites 13X and 5A, and metal-organic frameworks MIL-53(Al) and Fe-BTC.

All materials were analyzed at 30 °C while flowing an equimolar gas stream consisting of 10 sccm nitrogen and 10 sccm carbon dioxide. A 1 sccm stream of helium was also blended into the feed gas stream as a tracer gas to aid in identifying the start of the breakthrough experiment.

The breakthrough curves for the four materials are plotted below on a mass-normalized axis. The total quantity of CO₂ adsorbed follows the trend: molecular sieve 5A > zeolite 13X > Fe-BTC > MIL-53(Al).

The table below shows the total quantity adsorbed in mmol/g.

Material	Material carbon dioxide adsorbed
ZEOLITE 13X	2.94
MOLECULAR SIEVE 5A	3.52
MIL-53 (AI)	1.23
FE-BTC	2.30

Applications

Natural gas separation: Natural gas is a mixture of hydrocarbons and other gases that must be purified prior to use in industrial applications and households for heating and food preparation.

Direct air capture: DAC is difficult due to low concentrations of carbon dioxide in air along with other impurities including moisture, and the captured CO₂ may be sequestered underground, sold, or converted into value-added chemicals to offset carbon emissions.

CO₂ adsorption: Power generation, chemical plants, and refineries are significant point sources for carbon dioxide emissions and the higher concentrations often require different operating conditions when compared to direct air capture.

Olefin / paraffin separatons: Are a core part of the petrochemical industry and used to in the production of polymers such as polyethylene and polypropylene; these separations are energy intensive and increase CO₂ emissions.

Toxic gas adsorption: Porous solids are used for personal protection and also under development for the capture of toxic gases including sulfur dioxide, hydrogen sulfide, and nitrogen dioxide from natural gas or other process feeds.

Water adsorption: Harvesting water from the air may be a critical technology for many parts of the world clean, where the fresh water supply is limited due to an arid climate or the increasing usage of water for agriculture.

Zeolites: Pressure swing adsorption using Zeolite 5A, 13X, or LiX, which have high selectivity for adsorbing nitrogen are used commercially for air separation and producing oxygen.

Silicas: Amine functionalized silicas are effective and highly selective adsorbents and used for the direct air capture (DAC) of CO₂.

Porous membranes / monoliths: Porous membranes and monoliths coated zeolites or MOFs are commonly used to improve the operational efficiency of separation processes.

Activated carbon: Volatile organic component (VOC) from automobile fuel systems are captured by canisters filled activated carbon and these VOC emissions are minimized.

Porous aluminas: Alumina – Supported Ionic Liquids are effective adsorbents with potential applications for the separation of CO₂ from natural gas.

Metal-organic frameworks: MOFs are highly selective adsorbents which are effective for demanding commercial applications including alkanes & olefins, olefins & alkynes, DAC, CO₂ & CH₄.

Specification

General

Furnace	Maximum temperature: 1050 °C
Thermostated environmental chamber	Maximum temperature: 200 °C
Sample mass	Up to 2.5 g
Sample volume	Up to 2.5 mL

Additional specifications

Analysis	Determination of breakthrough curves: Programmable total pressure, flow rate, composition and temperature Investigation of kinetic performance of adsorbents: Optimised for research-scale sample sizes with interchangeable reactor beds Investigation of co-adsorption and displacement: Ultra-low dead volume for rapid signal response Determination of sorption selectivity: Automated switching between purge and process gases High-resolution separations using small sample quantities: Configurations for gas-vapor and vapor-vapor separation Dynamic adsorption and desorption experiments: Door remains locked during analysis to protect user and the analysis from altered temperature conditions Determination of single- and multi-component adsorption data: Touch Screen In-situ sample preparation up to 450 °C with a SS column and 1050 °C with a quartz column: Patented “No Dead Volume” mixing valve with rapid switching Fully automated control via PC: Up to 6 high precision mass flow controllers

Analysis

Determination of breakthrough curves: Programmable total pressure, flow rate, composition and temperature
Investigation of kinetic performance of adsorbents: Optimised for research-scale sample sizes with interchangeable reactor beds
Investigation of co-adsorption and displacement: Ultra-low dead volume for rapid signal response
Determination of sorption selectivity: Automated switching between purge and process gases
High-resolution separations using small sample quantities: Configurations for gas-vapor and vapor-vapor separation
Dynamic adsorption and desorption experiments: Door remains locked during analysis to protect user and the analysis from altered temperature conditions
Determination of single- and multi-component adsorption data: Touch Screen
In-situ sample preparation up to 450 °C with a SS column and 1050 °C with a quartz column: Patented “No Dead Volume” mixing valve with rapid switching
Fully automated control via PC: Up to 6 high precision mass flow controllers

Why Breakthrough Analyzer?

The Micromeritics BreakThrough Analyzer allows for the widest range of experimental conditions with unmatched automation from sample activation to analysis.

It offers several advantages over any competitive adsorption measurement system including:

Configurations with up to 2 vapor sources available
Proprietary zero-volume blending valves with unmatched minimization of dead times
Unparalleled touchscreen control
Thermostated environmental chamber delivers uniform temperature control up to 200 °C exclusive to the BreakThrough Analyzer
MicroActive software: the most intuitive, flexible, and comprehensive analysis software for adsorption studies

The Micromeritics BreakThrough Analyzer is capable of flowing up to two vapor streams simultaneously through its packed column. The thermostated environmental chamber prevents condensation of these vapor streams during analysis and ensures that all gases and vapors maintain a constant temperature within the instrument. Vapor streams are generated using a bubbler which allows for a carrier gas to reach saturation with the vapor of choice. The figure below displays multicomponent ethanol/water breakthrough measurements conducted on zeolite 13X.

[Micromeritics - Breakthrough-Analyzer - Multi component vapor analysis graphs.jpg] Micromeritics - Breakthrough-Analyzer - Multi component vapor analysis graphs.jpg

A safe and highly optimized device for collecting both transient and equilibrium adsorption data for multi component systems.

Automatic shut off from Software
Alarm in/out communication with central alarm system
Safety system separated from PC
Furnace temperature control alarm
Thermostated environmental chamber temperature control alarm
Full range of optional safety features available including automatic shut-off valves & gas detector

[Micromeritics - Breakthrough-Analyzer - safety - touch screen panel.jpg] Micromeritics - Breakthrough-Analyzer - safety - touch screen panel.jpg

MicroActive is the most intuitive, flexible, and comprehensive analysis software for adsorption studies

MicroActive Software allows for:

Data reduction from Mass Spectrometer
Quantity adsorbed & selectivity

The flexible, intuitive, easy-to-use software allows for the widest range of experimental conditions and automates the breakthrough from sample activation to sample analysis, including the ability to perform cyclic experiments. Paired with industry leading MicroActive analysis software, the BreakThrough Analyzer system accurately and reproducibly characterizes adsorbents, analyzes data with comprehensive analysis methods, and solves the breakthrough equation for the most demanding samples.

[Micromeritics BreakThrough Analyzer - software screen desktop.png] Micromeritics BreakThrough Analyzer - software screen desktop.png

Zeolite 13X has been extensively studied for applications in catalysis and adsorption. In this study, zeolite 13X was used as an adsorbent for carbon dioxide adsorption to collect breakthrough curves from 1 – 10 bar pressure.

These measurements were collected using equimolar flowrates of 10 sccm nitrogen and 10 sccm carbon dioxide. A 1 sccm stream of helium was used as a tracer gas to determine the start of the breakthrough experiment.

All measurements were collected at an analysis temperature of 30°C. Between each measurement, the zeolite 13X sample was reactivated overnight to ensure complete desorption of carbon dioxide. The figure shows a consistent increase in breakthorugh time across successive experiments as the pressure is increased.

Following carbon dioxide breakthrough measurements an equilibrium adsorption quantity was calculated for each curve by solving the breakthrough equation. Next, an isotherm was constructed displaying the quantity of carbon dioxide adsorbed at 1, 2, 3, 5, 7, and 10 bar total pressure. At 10 bar, zeolite 13X adsorbed roughly 15 mmol/g carbon dioxide. While isothermal data collected via breakthrough cannot be directly correlated with static adsorption measurements, it can provide a assessment of an adsorbent in process relevant conditions.

[Micromeritics - Breakthrough-Analyzer - high pressure adsorption graphs.jpg] Micromeritics - Breakthrough-Analyzer - high pressure adsorption graphs.jpg

System configurations

Mass Spectrometer: Multicomponent adsorption studies often require a mass spectrometer to monitor the residual gas composition. The MS is the most common detector system used for breakthrough analysis.

Fourier Transform Infrared (FTIR) analyzer: FTIR spectrometers are often selected for experimental breakthrough studies such as the separation of xylenes or other aromatic hydrocarbons.

Humidity sensor: Allows direct tracking of water content for low cost. This can be especially useful in production control applications.

Sample preparation system: Small quantities of active material can be mixed with an inert carrier to produce a homogeneous sample and improve analysis reproducibility.

CO₂ sensor: Allows direct tracking of CO₂ content for low cost. Can be especially useful in production control applications.

MFC and mixing valves (maximum 6 gas inlets): Additional mass flow controllers and blending valves may be added to the BreakThrough Analyzer to increase the analytical capabilities and expand the range of experiments that may be conducted.

Sample column (different volume): The BreakThrough Analyzer may be used with a variety of column diameters to accommodate different sample morphologies included powders, pellets, and extrudates.

Vapor source (max. 2): Moisture or other vapors such as xylenes or other aromatics are compatible with the optional vapor sources available for the BreakThrough Analyzer.

Enhanced chemical resistance: Special inert materials of construction enable simulation of process conditions – such as post-combustion CO₂ capture – that include highly reactive gases like NOx, H₂S, or SO₂.

User manuals

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Software downloads

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The superior selective adsorption system.

Compact, versatile, high performance adsorbent characterization. Enhanced operator safety features. Engineered for performance.