AutoChem III
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.
AutoChem III
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.
- Pulse Chemisorption
- TPR
- TPO
- TPD
- TPSR
- Dynamic B.E.T.
- Breakthrough Curve
- Metal Dispersion
- Metal Surface Area
- Active Surface Area
- Crystallite Size
- Heat Of Desorption
- Activation Energy
- B.E.T. Surface Area
- Metal-Supported Catalysts
- Acid or Base Catalyzed Reactions
- Oxide or Zeolite Catalysts
- Advanced Battery Anode Materials
- Fuel Cell Catalysts
AutoChem III Benefits
Quick & Easy
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 WITH AUTOCOOLÂ
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.
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NEVER PREPARE ANOTHER VAPOR CAPTURE SLUSH BATH
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. The NEW AutoTrap effectively traps vapor and requires no manual slush bath preparation.
Traditional methods for vapor capture require the time-intensive process of slush-bath preparation through the manual mixing of liquid nitrogen with isopropanol. The zeolite bed of the AutoTrap effectively captures vapors, can be used for several experiments without interruption and can be regenerated in situ.
PROGRAM WHAT YOU ENVISION, VISUALIZE WHAT YOU HAVE PROGRAMMED
The new MicroActive method editor features an intuitive process illustration that shows the programmed state of the instrument at every step of the method so you can see that your method matches your vision.
MAKING ACCURACY EASY:
EXCLUSIVE AUTOMATED DETECTOR CALIBRATION
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 WITH 18 AVAILABLE GAS STREAMS
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 you won’t compromise data accuracy by blending gases, which unnecessarily introduces errors from mass flow controllers.
Better Measurements
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.
PRECISION TEMPERATURE CONTROL
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
MOST ACCURATE GAS STREAM COMPOSITION
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.
And 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
SEE MORE OF YOUR REACTION WITH THE MOST SENSITIVE CHEMISORPTION SYSTEM IN THE WORLD
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 a 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.
CONTINUOUS CONTROLLED VAPOR DOSING
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..
MOVE QUICKLY FROM DATA TO DECISION
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
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
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 THIRD-PARTY TESTED AND VERIFIED
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. And 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
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.
AutoChem III Features
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AutoChem III Feature List
- Temperature-controlled corrosion-resistant detector is compatible with corrosive gases and inherently protected from gas leaks that can destroy alternative designs, providing high reliability and long operational life
- High sensitivity thermal conductivity detector (TCD)Â is 2x as sensitive as alternatives so you can measure smaller samples volumes, detect secondary reactions, and have greater confidence in your results
- 18 total gas inlets six each for preparation, carrier, and loop gases permit sequential experiments of different types and saves time between experiments
- Exclusive AutoTrap provides superior moisture removal for TPR experiments with a system that is effortless to use and saves hours per day 18 total gas inlets six each for preparation, carrier, and loop gases permit sequential experiments of different types and saves time between experiments
- Dynamic clamshell furnace provides temperature control up to 1200°C and controlled heating rates from 0.1°C/min to 100°C/min with the lowest available temperature overshoot
- Integrated AutoCool cools the furnace and sample quicker than forced air alone without the use of cryogenic liquids, saving an average of 30 minutes per experiment
- Internal gas temperature control in four separate zones prevents condensation during studies with vapor and improves overall signal stability
- The lowest internal gas volume provides the highest peak resolution and minimizes tailing when changing gas stream composition.
- KwikConnect retention system makes sample tube mounting quick, easy, and safe with no threaded connections and half as many separate pieces as traditional designs
AutoChem III Specifications
| 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 |
AutoChem III Capabilities
- Pulse Chemisorption
- Temperature-programmed reactions: TPR, TPO, TPD, TPSR
- Strong Chemisorption: Reactive metal area, dispersion, crystallite size
- Active site surface concentration
- Reduction, Oxidation Temperatures
- Acid site strength distribution: Lewis/Brønsted acid site distribution
- Breakthrough Curve Measurement
- Activation Energy
Optional Capabilities
- CryoCooler -100°C to 1200°C
- Detection by Mass Spec
- Continuous or Pulsed Vapor Dosing: water, alcohol, amines, aromatic organics, and more
- Enhanced Chemical Resistance
- B.E.T. Surface Area
Configurations
MASS SPECTROMETERÂ (MS)
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.
CRYOCOOLER
Begin experiments at temperatures as low as -100 °C with controlled liquid-nitrogen-based cooling.
VAPOR GENERATOR
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.
ENHANCED CORROSION RESISTANCE (ECR)
For reaction chemistries that requires 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 perfluoroelastomers, and inert-coated stainless steel to provide the greatest stability under the harshest working conditions.
Application & Methods
Applications
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Methods
TEMPERATURE PROGRAMMED REACTIONS
The suite of temperature programmed reactions are collectively used to measure reactivity as a function of temperature through change in gas stream composition. As temperature is increased, gas stream composition is changed through: consumption of reactive gases, creation of reaction products, and desorption of bound species.
TEMPERATURE-PROGRAMMED DESORPTION MEASUREMENT (TPD)
Species previously adsorbed can be desorbed by increasing sample temperature under flowing inert gas. Ammonia TPD is one of the most common applications. A sample is first saturated with ammonia during the preparation step, then heated to desorb bound ammonia, revealing relative acid site strength for materials such as zeolites. Similarly, desorption of carbon dioxide indicates the strength of basic sites. Bulk decomposition into the gas phase can also be used to characterize carbonates for CO2 removal or hydrides for hydrogen storage.
TEMPERATURE PROGRAMMED REDUCTION (TPR)
The TPR measurement is a specific case of temperature-programmed reaction in which a gas blend of hydrogen and an inert carrier – usually Argon – are passed over an oxide sample. Hydrogen is removed from the gas stream and water vapor is generated. The water vapor is trapped by the AutoTrap and the depletion of hydrogen from the carrier stream is measured. In particular, this measurement provides the required conditions (temperature, time, and activation energy) required to prepare a heterogeneous catalyst from its native oxide state into the active zero-valence metal.
TEMPERATURE PROGRAMMED OXIDATION (TPO)
In a TPO experiment, oxygen in the sample gas stream is consumed, generally reacting with different forms of carbon to produce CO or CO2. TPO experiments are important to characterize the reactivity of metal oxide catalysts and optimize process conditions. The temperature of oxidation is also associated with the reactivity of carbon-carbon bonds, and is therefore an effective means for differentiating forms of carbon. Using TPO, amorphous, nanotube, filament and graphitic carbon can be distinguished, especially those that form on catalysts.
PULSE CHEMISORPTION
A sample is prepared in situ to a known initial state (e.g. pure oxide or valence metal) through temperature and gas exposure. Reactive gas pulses of known volume are delivered across to the sample and the system measures the volume of gas consumed in each pulse.
B.E.T. SURFACE AREA: PHYSISORPTION
The AutoChem III can measure B.E.T surface area by the flowing or dynamic method in which N2 depleted from, or added to, a flowing gas stream is measured at liquid nitrogen, or ambient, temperatures, respectively. Basic physical surface area measurements are important for catalyst development as they reflect the basic physical form of the catalyst and/or support and the available contact area for reactivity. This is also an important basic measurement for porous and granular materials of all types.
BREAKTHROUGH CURVE ANALYSIS
Breakthrough analysis is a powerful technique for determining the adsorption capacity of a material under dynamic flow conditions. Breakthrough analysis allows users to precisely control temperature, pressure, and gas flowrates during an experiment. This allows users to analyze adsorbates under process relevant conditions, giving them the tools necessary to optimize their systems and adsorbent materials for their application. Additionally, breakthrough allows users to easily collect multicomponent equilibrium adsorption data allowing them to determine the selectivity and adsorption kinetics of their materials.
AutoChem III Resources
Application Notes
- Temperature-Programmed Reduction Using the AutoChem
- Characterization of Acid Sites Using Temperature-Programmed Desorption
- Accuracy of Vapor Dosing with the AutoChem
Standard Methods
- ASTMÂ D4824-94(1999):Â Standard Test Method for Determination of Catalyst Acidity by Ammonia Chemisorption
- ASTM WK17123: New Test Method for Test Method for Carbon Monoxide Chemisorption on Supported Platinum on Alumina Catalysts using Dynamic Flow Method
- ASTM WK71860: New Test Method for Acid Site Characterization on Zeolites Using Dynamic Flow Method
AutoChem III Photo Gallery
