Gas Sorptions – GAT Scientific http://staging.gatscientific.com Preferred Tools for Material Characterization Wed, 17 Jun 2020 05:45:16 +0000 en-US hourly 1 https://wordpress.org/?v=6.7.2 SAA 8100 http://staging.gatscientific.com/product/saa-8100/ Wed, 06 May 2020 02:19:49 +0000 /?post_type=product&p=1073

The quantity of gases adsorbed may be determined from a simple mass balance using the mass flow entering the column minus the mass flow of components exiting the column. This difference is the accumulation (adsorption) of components from the gas phase. The Selective Adsorption Analyzer is also often referred to as a Breakthrough Analyzer because of its ability to generate breakthrough curves.

Key Features and Benefits:

  • Optimized and minimized “dead volumes”
  • Simple column design with exceptional flow control enables multiple gases to be used with highly controlled blending
  • Sample column is housed in a precise, temperature-controlled hotbox, particularly important for Breakthrough experiments
  • Proprietary blending valves provide important advantages for gas mixing and for minimizing the system dead volume
  • System scalability that enables expansion of capabilities over time through addition of detectors and other optional accessories (e.g. Mass Spectrometer, GC/MS, Vapor generator, others available upon request)
  • Back pressure control that allows the user to perform experiments at commercially relevant conditions

Common Applications:

  • Gas separation, storage & purification
  • Breakthrough analysis
  • CO2 capture
  • Sorption selectivity
  • Evaluation of next generation adsorbent materials such as MOFs, COFs, ZIFs, zeolites, activated carbons, silica gels, activated alumina, molecular sieve carbon, porous polymers & resins

Common tests performed:

  • Multi component adsorption
  • Mixed gas adsorption
  • Breakthrough curve analysis
  • Adsorption of gas & vapor mixtures
  • Selectivity & adsorption capacity
  • Dynamic adsorption & desorption measurements
  • Competitive adsorption
  • High pressure isotherms
  • Pure component data (low pressure, high temperature, wide range of temperatures)

Carbon dioxide breakthrough curve using Basolite C300 (Cu-btc)

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HPVA II http://staging.gatscientific.com/product/hpva-ii/ Tue, 05 May 2020 14:14:37 +0000 /?post_type=product&p=1017

This process is repeated at given pressure intervals until the maximum preselected pressure is reached. Then the pressure can be decreased to provide a desorption isotherm. Each of the resulting equilibrium points [volume adsorbed and equilibrium pressure] is plotted to provide an isotherm.

Excellent reproducibility and accuracy are obtained by using separate transducers for monitoring low and high pressures.

HPVA II Benefits

  • Dual free-space measurement for accurate isotherm data
  • Free space can be measured or entered
  • Correction for non-ideality of analysis gas using NIST REFPROP compressibility factors calculated from multiple equations of state
  • Reports provided as interactive spreadsheets
  • Isotherm and weight percentage plots created automatically
  • Tables of raw data used for report calculations
  • Real-time charts for Pressure vs. Time and Temperature vs. Time
  • Gas mixtures with up to three components can be used
  • Kinetic data provided for rate of adsorpotion calculations
  • Langmuir equation used to model Type I isotherms
  • High-precision, solid-state design high-pressure transducer provides a reading accuracy of ±0.04% full scale with a stablility of ±0.1%
  • Low-pressure pressure transducer provides a reading accuracy of ±0.15% of value
  • System can attain a maximum pressure of 200 bar
  • Hydrogen gas sensor automatically shuts down the system should a hydrogen leak occur
  • BET surface area, Langmuir surface area, and total pore volume calculations included

Specification

Physical
  • Height 88.9 cm (35 in.)
  • Width 50.8 cm (20 in.)
  • Depth 50.8 cm (20 in.)
  • Weight 27.2 kg (60 lbs.)
Electrical
  • Voltage 100 – 240 VAC.
  • Frequency 50 – 60 Hz.
Temperature
  • 10 to 45 °C (50 to 113 °F.)
  • 10 to 55 °C (14 to 131 °F.)
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ASAP2050 http://staging.gatscientific.com/product/asap2050/ Mon, 04 May 2020 04:20:27 +0000 /?post_type=product&p=723

Knowledge of chemical reactivity and material properties, particularly with respect to exposure under different conditions (air, moisture, etc.) needs to be gathered.

Micromeritics’ ASAP 2050 Xtended Pressure Sorption Analyzer is designed to address these and many other elevated-pressure sorption needs. The instrument combines many of the capabilities of Micromeritics’ popular ASAP 2020 with additional features that allow the user to obtain data in an extended-pressure environment.

Standard ASAP Features
  • Two independent vacuum systems allowing simultaneous automated preparation of two samples and analysis of another
  • Two-station intelligent degas system for fully automated degassing with precisely controlled heating profiles
  • A highly flexible and interactive reporting system that includes an extremely versatile graphic user interface allowing custom presentation of results
Additional ASAP 2050 Features
  • Analysis System
  • Analysis manifold is capable of operating from vacuum to 10 atmospheres
  • An optional chiller Dewar and recirculating bath allow the ASAP 2050 to be operated indefinitely – the instrument also supports the use of a standard Dewar with cryogen (typically liquid nitrogen or argon) that will provide at least 50 hours of unattended analysis without refilling the Dewar
  • Straight-walled, stainless-steel sample tubes are capable of safe operation up to 150 psia
  • Rapid collection of non-monotonic isotherms with standard isotherm cycling software
  • Special degas heating mantles can be used to prepare samples in situ on the analysis port prior to analysis
  • Degas System
  • Temperatures at each degas port, and the rate of temperature change, can be set and monitored individually from a few degrees above ambient to 450 oC
  • A user specified pressure setting protects the sample from steaming or damage during sample preparation.

ASAP 2050 Hardware Advantages

The ASAP 2050 uses two independent vacuum systems, one for sample analysis and one for sample preparation. This allows preparation and analysis to proceed concurrently without the inherent delay found in single vacuum system analyzers that must share a pump. Moreover, independent systems completely eliminate the possibility of cross-contamination between the degas and analysis manifolds.

A two-station intelligent degas system provides fully automated degassing with controlled heating time profiles. Temperatures at each degas port, and the rate of temperature change, can be set and monitored individually. The temperature can be controlled from a few degrees above ambient to 450 ºC. A sample may be added to or removed from a degas port without disturbing the treatment of the other sample. The degas treatment information is saved as part of the sample file, included in analysis reports, and can be conveniently copied and reused for other samples to ensure repeatability and reproducibility.

Stainless-steel, temperature-monitored analysis manifolds are designed for optimal internal volumes and superior vacuum performance. These optimized manifolds, in combination with temperature monitoring, ensure highly accurate measurements of sorbed gas volumes. Analysis manifolds are capable of operating from vacuum to 10 atmospheres. This allows a rapid collection of isotherms.

An optional chiller Dewar and recirculating bath allow the ASAP 2050 to be operated indefinitely. The instrument also supports the use of a standard Dewar with cryogen that will provide at least 50 hours of unattended analysis without refilling the Dewar. Micromeritics’ patented Isothermal Jackets can be used to assure a constant thermal profile along the full length of both the sample and saturation pressure (P0) tubes throughout extended analyses.

ASAP 2050 Stainless-Steel Sample tube

Straight-walled, stainless-steel sample tubes enable extended pressure analyses and are capable of safe operation up to 150 psia (10 atmospheres).

The ASAP 2050 features a single high-quality, stable, low-noise transducer system for all measurements. This eliminates the possibility of progressive offset and drift between separate transducers covering the same range.

Special degas heating mantles can be used to prepare samples in situ on the analysis port prior to analysis. The new heating mantle is designed to allow the user to place the mantle on the sample tube without removing the Dewar.

ASAP Reference Materials

Lanthanum Penta-Nickel (LaNi5)

is a well-known alloy that readily forms hydrides. This reference material is recommended for use with the ASAP 2050 to demonstrate the formation and characterization of hydrides. This material is ideally suited for use with the pressure composition isotherm report.

Silica-Alumina

is a typical porous, high surface area reference material. The surface area of the silica-alumina typically exceeds 200 m2/g and the pore size is a nominal 100 Å. This material is recommended for users who analyze amorphous materials with surface area ranging from 10 to greater than 300 m2/g for both non-porous and porous materials in the 40 – 3000 Å range. Silica-alumina is suitable for use with BET, t-plot, and BJH pore size reports.

Carbon Black

Standard Reference Blacks are available from 20 to greater than 100 m2/g and are stable, well-characterized materials. They are recommended for all users but may be especially suited for researchers in the carbon, tire, and filler industries. Carbon black reference materials are suitable for use with BET and STSA reports.

Glass

A 5 m2/g glass reference material is recommended for industries and users who characterize materials in the 1 through 50 m2/g range. Glass reference material is suitable for use with BET surface area reports.

ASAP 2050 XP Software Features and Reports

The easy-to-use ASAP 2050 software utilizes a Windows interface that includes Wizards and applications to help plan, launch, and control the analysis. You can collect, organize, archive and reduce raw data, and store standardized sample information and analysis conditions for easy access during later applications. Finished reports may be generated to screen, paper, or data transfer channels. Features include cut-and-paste graphics, scalable-and-editable graphs, and customizable reports.

Additional capabilities include:
  • Degas temperature profiles and treatment time data are integrated with the sample file for future reference and verification of SOP compliance.
  • The Instrument Schematic screen displays the instrument’s current operating status, including the real-time isotherm, and allows the operator to assume manual control of the instrument if desired.
  • One computer can control two Micromeritics ASAP analyzers of the same or different model making efficient use of valuable lab space. Other types of Micromeritics instruments can also be connected.
  • Up to nine graphs can be overlaid for easy comparison of different samples or for comparison of different data reduction techniques applied to the same sample.
  • Exportable data tables provide for merging and comparing data from other sources in a unified single spreadsheet file.
  • Three modes of gas dosing routines provide effective choices to ensure maximum speed with full accuracy for samples with widely differing isotherm shapes.
  • The patented Smart Dosing™ routine actually learns about the sample’s potential to adsorb gas and adjusts the adsorptive doses accordingly. This helps prevent over-dosing the sample and obscuring porosity information.
Analyses and Reports

The ASAP 2050 includes powerful data reduction software to provide a variety of easy-to-interpret report options. This allows tremendous flexibility in the selection of analysis constants to best fit your specific application. All ASAP models have the capability to collect data over a prescribed segment of the pressure range, or to perform adsorption and desorption analyses over the entire pressure range, providing extensive surface area and porosity information. The ASAP 2050 is a versatile adsorption instrument. In addition to collecting adsorption isotherms up to 150 psia, traditional isotherms may be collected with nitrogen; BET surface area and BJH pore size distributions are easily determined.

The ASAP 2050 model includes:

  • Repetitive Isotherm Cycling
  • DFT (Density Functional Theory)
  • Single- and Multipoint BET (Brunauer, Emmett, and Teller) surface area
  • Langmuir surface area
  • Temkin and Freundlich isotherm analyses
  • Pore volume and pore area distributions in the mesopore and macropore ranges by the BJH (Barrett, Joyner, and Halenda) method using a variety of thickness equations including user-defined, standard isotherm
  • Pore volume and total pore volume in a user-defined pore size range
  • F-Ratio plots that illustrate the difference between theoretical and experimental isotherm data
  • Heat of Adsorption

The ASAP 2050 is a versatile adsorption instrument. In addition to collecting adsorption isotherms up to 150 psia (top), traditional isotherms may be collected with nitrogen (middle); BET surface area and BJH pore size distributions are easily determined (bottom).

Hydrogen isotherms at several temperatures are rapidly measured using the ASAP 2050.

The Pressure Composition Isotherm of lanthanum nickel demonstrates the ability to characterize hydride formation using the ASAP 2050.

High-resolution nitrogen and oxygen isotherms for pressure-swing adsorption applications are easily obtained using the ASAP 2050.

ASAP2050 XP Technique Overview

The basics of the analytical technique are simple; a sample contained in an evacuated sample tube is cooled (typically) to cryogenic temperature, then is exposed to analysis gas at a series of precisely con-trolled pressures. With each incremental pressure increase, the number of gas molecules adsorbed on the surface increases. The pressure at which adsorption equilibrium occurs is measured and the universal gas law is applied to determine the quantity of gas adsorbed.

As adsorption proceeds, the thickness of the adsorbed film increases.Any micropores in the surface are quickly filled, then the free surface becomes completely covered, and finally larger pores are filled.The process may continue to the point of bulk condensation of the analysis gas. Then, the desorption process may begin in which pressure systematically is reduced resulting in liberation of the adsorbed molecules. As with the adsorption process, the changing quantity of gas on the solid surface is quantified. These two sets of data describe the adsorption and desorption isotherms. Analysis of the isotherms yields information about the surface characteristics of the material.

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