Autochem III - Catalyst Characterization Analyzer

A catalyst characterization laboratory in a single analytical instrument

Industry-leading accuracy through superior sample and gas temperature control, patented gas blending, and 100% sensor sensitivity improvement
Save hours per day with rapid cooling, a non-cryogenic moisture trap for TPR, and the most available pre-plumbed gas streams
Enhance operator safety by operating without glass vacuum dewars, cryogenic liquids, or complicated operations with hot fittings

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Overview

The AutoChem from Micromeritics is the most widely used and highly cited system for catalyst reactivity characterization because it is also the most automated, highly accurate system for chemisorption and temperature-programmed reactions.

The all-new AutoChem III meets and exceeds that performance with a design that will save you hours a day, make the most sensitive, reproducible measurement, and enhance operator safety.

Applications

Net zero technologies: The development of efficient and effective catalysts is necessary to the continued development of CO₂ mitigation and the hydrogen economy that will enable a sustainable energy future. The AutoChem III is a useful tool to optimize adsorption and dissociation of H₂/O₂ on electrolysis electrodes, show whether desorption occurs near reaction conditions, quantify acid or base sites to optimize reactivity and selectivity, and more.

Fuel cells: Platinum-based catalysts including Pt/C, PtRu/C, and PtRuIr/C are often characterized by temperature-programmed reduction to determine the number of oxide phases and pulse chemisorption to calculate: metal surface area, metal dispersion and average crystallite size.

Partial oxidation: Manganese, cobalt, bismuth, iron, copper, and silver catalysts used for the gas-phase oxidation of ammonia, methane, ethylene, and propylene are characterized using temperature-programmed oxidation and desorption, heat of desorption & dissociation of oxygen.

Catalytic cracking: Acid catalysts such as zeolites are used to convert large hydrocarbons to gasoline and diesel fuel. The characterization of these materials includes ammonia chemisorption and temperature-programmed desorption.

Catalytic reforming: Catalysts containing platinum, rhenium, tin, etc. on silica, alumina, or silica alumina are used for the production of hydrogen, aromatics, and olefins.

Isomerization: Catalysts such as small-pore zeolites (mordenite and ZSM-5) containing noble metals (typically platinum) are used to convert linear paraffins to branched paraffins.

Hydrocracking: Hydrodesulfurization and Hydrodenitrogenation: Hydrocracking catalysts typically composed of metal sulfides (nickel, tungsten, cobalt, and molybdenum) are used for processing feeds containing polycyclic aromatics that are not suitable for typical catalytic cracking processes.

Water gas shift reaction: The water-gas shift reaction is an important element in the hydrogen lifecycle and the push toward net-zero technologies. The combination of catalysts, often copper-zinc-alumina and iron-chromia, are characterized by TPR and pulse chemisorption to maximize activity.

System configurations

Mass spec provides a direct probe for the identity and quantity of specific reaction products. This is especially valuable when investigating an unknown reaction, or a reaction that creates multiple products. The single quadrupole mass spec with heated transfer line provides detection of mass fragments up to 200 amu and data collection that is integrated with the operation of the AutoChem III. The AutoChem III also includes a general mass spec communication port for coordination with a lab’s existing mass spec.

Prepare samples for analysis or perform measurements in the presence of pulsed or continuous vapor streams such as water, alcohol, pyridine, aromatic organics, and more.

Begin experiments at temperatures as low as -100 °C with controlled liquid-nitrogen-based cooling.

For reaction chemistries that require particularly aggressive gas compositions, a special version of the AutoChem III is available with enhanced corrosion resistance. Wetted materials are constructed from highly resistant Hastelloy, highly stable perfluoro elastomers, and inert-coated stainless steel to provide the greatest stability under the harshest working conditions

Specification

Temperature	Ambient to 1200 °C
Temperature ramp rates	-100 °C to 800 °C: up to 100 °C/min 800 °C to 1000 °C: up to 50 °C/min 1000 °C to 1200 °C: up to 25 °C/min
Preparation gases	6 inlets: H₂, O₂, He, Ar, H₂/Ar, and more
Carrier gases	6 inlets: He, Ar, H₂/Ar, and more
Analysis (loop) gases	He, H₂, CO, O₂, N₂O, NH₃/He, and more

Temperature

Ambient to 1200 °C

Temperature ramp rates

-100 °C to 800 °C: up to 100 °C/min

800 °C to 1000 °C: up to 50 °C/min

1000 °C to 1200 °C: up to 25 °C/min

Preparation gases

6 inlets: H₂, O₂, He, Ar, H₂/Ar, and more

Carrier gases

6 inlets: He, Ar, H₂/Ar, and more

Analysis (loop) gases

He, H₂, CO, O₂, N₂O, NH₃/He, and more

Quick & easy

The new AutoChem III is designed to make key operations quick and easy, saving you hours a day so you can spend less time making measurements and more time making progress.

Rapid turnaround time

The NEW AutoCool is an integrated gas-fed system that rapidly cools sample tubes before and during experiments.

AutoCool is typically 30 minutes faster than alternative systems and requires no liquids or external support.

Never prepare another vapor capture slush bath

The NEW AutoTrap effectively traps vapor. Simple and effortless to use, the AutoTrap can save hours of preparation time each day.

The AutoTrap requires no manual slush bath preparation.

Visualize your methods

Program what you envision, visualize what you have programmed.

The NEW MicroActive method editor features an intuitive process illustration for methods on the AutoChem.

Utilise visual process illustrations which show the programmed state of the instrument at every step of the method - so you can ensure your method matches your vision.

Making accuracy easy

The AutoChem III makes quantitative accuracy simple with automated detector calibration. Traditional systems require calibration by multiple runs of reference materials or single-point offsets that ignore changes in temperature or pressure.

The AutoChem III generates accurate results through a fully automated process using the system’s patented gas blending capabilities including compensation for injection loop temperature and pressure to ensure the highest calibration – and result – accuracy. The process is fast, automated, requires no operator intervention, and produces more accurate results than alternative designs.

US Pat #10,487,954 B2

Loading samples is a snap

The patented NEW KwikConnect makes sample tube installation faster, easier, and more reliable than traditional designs with half as many separate pieces and no threaded fittings. Installation and removal are easier and quicker, reduce the risk of breaking sample tubes, and provide peace of mind that the snap lock closure has completely sealed the system.

US PAT #11,105,825 B2

Ready to run

Don’t waste time reconnecting and switching gas lines: have what you need ready when you need it. The AutoChem III has 18 available gas streams so you’re always ready to run your next reaction.

Having the right blended gas ready also means you won’t introduce errors from poorly designed external gas connections, and won’t compromise data accuracy by blending gases, which unnecessarily introduces errors from mass flow controllers.

Better measurements for more confident decisions

The AutoChem III provides results that drive confident decisions. The highest available measurement accuracy and repeatability – made under conditions that match your reaction environment – give you certainty to act with confidence.

Exacting thermal accuracy is essential to simulate reaction conditions while preventing the deactivation of precious catalyst materials. The AutoChem III exceeds all available systems in every key performance characteristic:

Widest range of temperatures: -100 °C to 1200 °C
Widest range of heating rates: 0.1 °C/min to 100 °C/min
- Repeatable temperature profiles
- Accurate determination of activation energy, Ea
Local sample temperature measurement
- Superior control accuracy without overshoots
Four independently controlled gas stream temperature zones eliminate vapor condensation and enhance measurement stability

The AutoChem III features the lowest gas flow path volume to eliminate carryover and signal tailing when changing gas flow conditions. This guarantees precise gas stream composition, even when switching configurations from one experiment to another.

With 18 available gas inlets, you will have the gas composition that you need ready, without introducing errors associated with blending gases in situ.

Better Temperature Control at Every Step

Furnace: to simulate reaction conditions
Vapor: to control vapor composition
Gas stream: to maximize detection sensitivity
Detector: to ensure robustness

The new AutoChem III features a new thermal conductivity detector (TCD) that is 110% more sensitive than previous designs. This enables you to use lower sample masses, accurately detect secondary reactions, and achieve greater accuracy of catalyst traits like site coverage.

Detector sensitivity is enhanced by a reference stream with a dedicated mass flow controller (MFC) that provides a stable reference to the sample stream. Alternative designs use a common carrier stream for both the reference and signal paths, resulting in interference between the measurement and reference stream leading to signal instability.

The temperature-controlled TCD is a robust sensor with long operating life and intrinsic protection from operational errors like gas flow leaks that cause premature failure of 4-element detectors used in inferior designs.

Achieve faster analysis and more complete characterization of surface selectivity and functionality with the available vapor generator featuring automated vapor calibration, injection repeatability better than 1%, and all new continuous dosing capabilities.

This system creates uniform streams of saturated vapors such as water, alcohols, amines, or organics that are used to prepare samples for TPD or as the reaction gas stream.

The new continuous dosing capability enables faster and more uniform vapor dosing than legacy systems that are limited to discrete vapor stream pulses.

Rapidly transition from experimental data to material characteristics with Micromeritics’ own AutoChem data analysis software. Get all the answers you need with:

Interactive peak analysis including limit selection, baseline definition, integration, and deconvolution
Built-in analysis models for pulse chemisorption, % dispersion, metal surface area, crystallite size, first-order kinetics, heat of desorption, activation energy, BET, Langmuir, total pore volume, and more
Seamless integration of mass spec data
Detailed, configurable graphical reports

Improving operator safety

The AutoChem III enhances operator safety at every stage of the measurement, reducing opportunities for exposure and potential for hazardous conditions.

No cryogenic liquids

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The new AutoTrap removes moisture without cryogenic liquids such as liquid nitrogen. The AutoTrap also eliminates the need for slush bath preparation, which requires vigorous mixing of alcohols and other solvents in glass vacuum flasks.

Cool to the touch

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The new AutoCool brings sample tubes to room temperature so fast after every experiment that you can change samples and start the next experiment quickly, without handling hot glass sample tubes. The KwikConnect sample tube retention system allows you to release the tube in one motion without fumbling with threaded connections and separate adapter pieces.

Third-party tested and verified

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Micromeritics products are third-party-tested to conform to the highest level of regulatory compliance and operational safety. Install and run with the confidence that the system will meet or exceed requirements for electrical safety and compatibility with the need for separate qualifications or assessments.

Micromeritics AutoChem III