Gravimetric Analysers for the Characterisation of the Sorption Properties of Materials.

Transcription

1 Gravimetric Analysers for the Characterisation of the Sorption Properties of Materials.

2 + - IGA - The Intelligent Gravimetric Analyser The IGA range from Hiden Isochema provides the ultimate tool for sorption science... The IGA system uses the gravimetric technique to accurately measure the magnitude and dynamics of gas and vapour sorption on materials. The IGA design integrates precise computer-control and measurement of weight change, pressure, temperature, gas flow and composition. The system can automatically and reproducibly measure sorption isotherms/isobars as well as investigating thermal desorption in diverse operating conditions. The unique IGA method exploits the relaxation behaviour of the interaction process after pressure/gas composition/temperature changes to simultaneously evaluate kinetic parameters and the asymptotic uptake. An uncompromising attitude to system design coupled with our experience in solving problems in sorption science in some of the most prestigious laboratories around the world makes Hiden Isochema the obvious and only choice for a sorption analyser. Microprocessor Thermostatted Microbalance Pressure Controller Wall Mounting Bracket INTELLIGENT GRAVIMETRIC ANALYSER Gas/Vapour Delivery: High pressure gases Vapours Gas/Vapour mixtures C T P M COM ISOCHEMA ISOCHEMA ANTI-CONDENSATIONSYSTEM Vacuum Pump Isolation Valve Vacuum/Pressure Vessel Sample Environment: Furnace Water bath Dewar Sample (internal temperature probe) All IGA models incorporate the following features: Ultra-sensitive microbalance mounted in thermostatted heatsink to provide high resolution and precise long-term stability. Pressure vessel incorporating all-metal seals designed to UHV standards to allow measurements from high vacuum to high pressure. Basic models can be upgraded to extend their range of applications, as your research program develops. State-of-the-art pressure control system capable of accurately controlling the pressure of gases and vapours across eight decades of pressure measurement. Versatile temperature controller for ramp and set-point operations in the temperature range from cryogenic to 1 C. Internal temperature probe to measure sample temperature. Full automation and extensive software package for experiment design, system control, data acquisition/archival, analysis and export. Unique and innovative approach for the determination of the sorption kinetics and equilibrium isotherms - The IGA method. Complete range of accessories including vacuum pumping stations, furnaces, humidifier, water baths etc. to enable a broad range of experiments to be performed.

3 The IGA Method Weight Pressure Pn En Pressure/gas composition is changed and then held constant during sorption at the set point P n. Weight data is acquired and analysed in realtime to determine kinetic parameters and predict the exact point of equilibrium uptake E n. Time Uptake En Equilibrium points are collected and plotted as an isotherm. The IGA method provides a consistent reproducible analysis method pointto-point on the isotherm whilst making the optimum use of laboratory time. Pn Pressure IGA-1 Gas Sorption System The IGA-1 system is specifically designed as a versatile gravimetric analysis system. The system can be configured to study general gas sorption processes from vacuum to high pressure as well as being used as a high pressure thermobalance with mass spectrometer interface (IGA-DSMS). Typical Application Materials Gas sorption Zeolites Sorption kinetic analysis Carbons Outgassing behaviour Metal/intermetallic hydrides TG studies High T c materials/ceramics In-situ surface area analysis Polymers In-situ pore size analysis 4 Comparison of nitrogen and oxygen adsorption on 5A Zeolite 14 Kinetics of R-134A sorption on carbon Nitrogen Oxygen Weight Change (g) m(t)=m + m[1-exp(-kt)] m = 55 µg m = 838 µg k = 3. x 1-4 s Pressure (Bars) Time (Minutes) The IGA-1 system can be used to determine the gas sorption properties of porous materials such as zeolites. The data shows a comparison between the oxygen and nitrogen sorption on a 5A zeolite up to an equilibrium pressure of 1 bars. The kinetic response shown above (the IGA method) is used to determine equilibration. Such data can prove useful in understanding the non-equilibrium sorption behaviour of materials in order to determine diffusion and transport parameters of adsorbates in materials. The example above shows a kinetic response for the sorption of a freon on activated carbon.

4 IGA- Vapour Sorption System The IGA- system is specifically designed to study general vapour sorption processes from vacuum. This model includes all the features of the IGA-1 model but additionally incorporates anti-condensation protection rated to 5 C. An additional low range pressure sensor is included. The system can be fitted with a UHV pump isolation valve to achieve the best possible vacuum at the sample position and a vapour delivery system is incorporated with the pressure controller. The IGA- can be used to study water and hydrocarbon vapour sorption on porous materials such as pharmaceuticals, carbons, catalysts, zeolites, clays and polymers. The IGA- vapour delivery and pressure control system. A broad range of liquids can be used in the reservoir to generate the vapour adsorbate. Water sorption on polymer paint film Hydrocarbon sorption on ZSM C 7.1C 4.4C.8C.3C Cyclohexane Benzene Mesitylene Pressure (Millibars) The IGA- system can be used to determine the water sorption properties of porous materials such as polymers and zeolites. The data shows isothermal uptake curves measured at closely separated temperatures between C and 3 C on a polymer paint film Pressure (Millibars) The IGA- system can be used to measure hydrocarbon vapour sorption on porous materials. Such data can be used to determine sample properties such as pore size from adsorbate molecular dimensions. IGA-3 Multi-component Sorption System The IGA-3 system is designed to study multi-component gas and/or vapour sorption processes from vacuum to high pressure. The system incorporates a multiple inlet mass flow control system. An internal gas delivery system injects the gas stream below the sample and extracts above enabling a defined gas composition to be established at the sample position. Flow and pressure control are independent allowing different gas compositions to be generated at different pressures. A balance purge can be provided in this system to allow the use of corrosive gases/vapours at the sample position while protecting the integrity of the weighing system. The system can be interfaced with a humidifier or vapour generator to define vapour compositions in the sample reactor. The IGA-3 system can be used to study multi-component gas/vapour sorption on materials such as carbons, zeolites, polymers and catalysts. The IGA-3 gas injection/exhaust system. Up to four gas streams can be mixed prior to injection into the sample CH 4 -CO Dual component isotherms on carbon at 5 C Air/Freon Mixture - adsorption isotherms on activated carbon 6 /1.5 4 C 5 Ratios indicated as CH4/CO. O 55 C 7 C 85 C Weight (Micrograms) 4 3 5/75 5/5 75/5 Amount Adsorbed (g/g) C 15 C 15 C 1 1/ Pressure (Millibars) The IGA-3 system can be used to determine multi-component gas sorption isotherms. The data above shows the binary isotherm for carbon dioxide and methane measured on carbon. Each isotherm was obtained at a constant gas composition. It is similarly possible to measure a composition scan at constant pressure Pressure (Bar) The data shows multi-component isotherms for a freon/air mixture of 4% on an activated carbon. Such information is required when designing filtration systems.

5 IGASORP Moisture Sorption System The IGASORP system is specifically designed to study the moisture sorption properties of materials. The system uses the same operating principles as in the rest of the IGA range. This system is used to model technological applications where moisture behaves as a critical component in either formulation, production or storage. The fully automated benchtop analyser offers superior performance and flexibility than traditional methods of moisture analysis while dramatically reducing analysis times. Typical Application Materials Moisture sorption isotherms Pharmaceutical formulations Hydration/dehydration studies Excipients, whole tablets Permeation studies Packaging materials QA/QC of raw/finished materials Building materials.5 Aspirin Moisture sorption on aspirin/blister pack 6 Permeation of moisture through blister packaging in atmosphere of 9% RH at 3 C Empty blister Weight change (microgrammes) %-RH (%) Time (Hours) The IGASORP system can be used to determine the moisture sorption properties of pharmaceutical materials. The data above shows the comparative reactions for an Aspirin tablet and it s blister packaging material. The IGASORP system can be used to study the permeation properties of packaging materials. Such studies prove invaluable in determining the effectiveness of storage media and the shelf-life of hygroscopic materials. IGA-PTCS Pressure/Temperature control system The IGA-PTCS system adds a pressure/flow and temperature control interface to existing microbalance systems. The upgraded system has all the functionality of the IGA range including the IGAS applications software. Microbalance systems such as Cahn and Sartorious can be easily interfaced providing full automation. The IGA-PTCS components consists of: Pressure control to bar. Temperature control of a wide variety of furnaces to 1 C. Four stream mass flow control system. IGAS applications software. IGA-DSMS Mass Spectrometer system Hiden s range of mass spectrometers can be interfaced to all of the IGA models. The IGA-DSMS combines the gas and gravimetric analysis techniques to provide an invaluable tool in materials characterisation. The system can be used to study thermal decomposition and desorption processes. Broad AMU range with triple mass filter options. Heated capillary transfer. Bypass pumping arrangement for rapid response time. Automated control from IGAS software. Mobile cart for stand-alone operation. Accessories A complete range of accessories and stand-alone modules are offered to supply complete turn-key solutions. These include: Complete range of furnaces from set-point control to high temperature TG applications. Liquid nitrogen control systems. Water baths for stable ambient temperature control. Humidifier module for relative humidity control. Vacuum pumping stations. Stand-alone vacuum/pressure microbalance system with data logging software.

6 Specifications Models IGA-1, IGA- and IGA-3 Weight Balance Capacity*: 5 grams Weighing Range*: Typically mg Resolution:. µg Long term stability: +/- 1 µg Sample containers: Glass/quartz/ceramic/steel mesh * Larger balance capacities and ranges available Pressure Vessel: Design pressure: Design temperature: Pressure sensors: Control accuracy: Temperature Pressurised-UHV SS316/SS34 assembly bars 5 C at pressure 1 C with quartz reactor (ambient pressure) Up to three per system ranging from 1 mbar to bar +/-.5% of transducer span (i.e..5 mbars for 1 bar transducer) Sensors: Type K or platinum resistance thermometers Range: Liquid nitrogen to 1 C Control accuracy: +/-.5% to +/- 1 C depending on control equipment ACS: 5 C Anti-condensation protection (IGA-) Flow Control (IGA-3) Flow rate: No. of streams: 5 ml/min (standard configuration) Up to four Optional balance purge for corrosive gases IGASORP Weight Balance Capacity*: 5 grams Weighing Range*: 1mg/mg/5mg Resolution:.1 µg for 1mg range Long term stability: Nominal +/- 1 µg/week Sample containers: Glass/steel mesh * Larger balance capacities and ranges available Humidity Sensor accuracy: Sensor response: Control range: Regulation accuracy: Gas: Max. flow rate: Temperature +/- 1% (-9%RH) +/- % (9-1%RH) 15 seconds to 9% of reading %RH (determined by gas supply) to 95% RH +/-.1% RH Typically dry air or nitrogen 5 ml/min Bath thermostat: Measurement range: 5 C to 85 C Accuracy/stability: +/-.5 C to +/-.1 C across range Internal heater for rapid drying: Max. temperature: 35 C Max. heating rate: 1 C/min More detailed specifications for the complete IGA range can be obtained from the relevant Technical Data Sheet (see below) The Sorption Products Range IGA-1 Gas sorption studies from vacuum to bar. IGA- Vapour sorption studies from vacuum incorporating anti-condensation protection. (Technical Data Sheet 137) IGA-3 Dynamic multi-component gas/vapour sorption incorporating gas flow controller. (Technical Data Sheet 138) IGASORP Benchtop system for analysing the moisture sorption properties of materials. (Technical Data Sheet 143) IGA-PTCS Pressure/flow/temperature control system for upgrading existing microbalances. (Technical Data Sheet 139) IGA-DSMS Mass spectrometer interface for gas analysis can be interfaced to all IGA models. (Technical Data Sheet 14) HP-ABR Automated high-pressure breakthrough rigs for characterization of sorbent materials Additionally, Hiden can supply stand-alone microbalance systems for vacuum or high pressure with data logging/control software. If you require further, more detailed information on any of the product range, please request the appropriate Technical Data Sheet (provided above) and our experienced staff will be happy to provide these details and discuss your specific experimental applications. Manufactured in England by: ISOCHEMA HIDEN ISOCHEMA LTD 31 EUROPA BOULEVARD WARRINGTON WA5 7TN ENGLAND Tel: +44 () Fax: +44 () info@hidenisochema.com Web: Certificate No It is Hiden Isochema s policy to continually improve product performance and therefore specifications are subject to change. TECHNICAL DATA SHEET 146 Printed in England