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INVERSE GAS CHROMATOGRAPH
The world’s most advanced
being the reverse of a conventional gas chromatographic (GC) experiment. and the time taken for the pulse or concentration front to elute down the column is measured by a detector.g.SURFACE MEASUREMENT SYSTEMS s m s GC Advanced instrumentation for the characterisation of particulates. The principles of IGC are very simple. The unique SMS flow control CONTROL PC technology* provides the stateof-the-art in humidity control together with unrivalled accuracy and reproducibility. A cylindrical column is uniformly packed with the solid material of interest. The standard instrument configuration comes with a thermal conductivity detector (TCD) and a flame ionization detector Carrier gases (FID): this combination allows differentiation between moisture Flow and organic solvent elutants. fibre or film. ANALYTICAL GAS CHROMATOGRAPHY Sample gas pulse Standard analytical column packing Separated sample peaks INVERSE GAS CHROMATOGRAPHY (IGC) Single probe gas pulse Packed sample column (particulate or fibre) Single peak (Retention time t R ) I N T R O D U C I N G T H E R E V O L U T I O N A R Y S M S iG C Column Packed sample T * patent applied for he revolutionary iGC from SMS SMS iGC SCHEMATIC is the world’s first commercial inverse gas chromatograph. Further control module detectors may be added Probe gas and humidifier (e. FID TCD Flow switching module Column module Detector modules PROBE GAS OVEN COLUMN OVEN . A series of IGC measurements with different gas phase probe molecules then allows access to a wide range of physico-chemical properties of the solid sample. Mass Spectrometer) according to customer module requirements. fibres and thin-films. typically a powder. W H A T I S I N V E R S E G A S C H R O M A T O G R A P H Y (I G C) ? I nverse Gas Chromatography (IGC) is a gas-phase technique for characterising surface and bulk properties of solid materials. A pulse or constant concentration of gas is then injected down the column at a fixed carrier gas flow rate. Opening up a whole new world of sorption solutions.
These properties can provide valuable insight into particular process or performance-related issues.g. Effect of Surface Modification Treatments Competitive Adsorption e.g. Surface Characterisation of Catalysts Surface Adsorption Isotherms at Low Concentration e. The specially designed quick-change column fittings allow rapid changeover of samples while ensuring the integrity of the column seals. Pharmaceutical Inhalation Formulation Specific Polar Interactions e. Adsorption on Porous Materials Surface Heterogeneity e. Flexible and Powerful Characterisation Tool The SMS IGC instruments are designed with flexibility in mind.iG C I N S T R U M E N T K E Y B E N E F I T S Unprecedented Accuracy and Repeatability The combination of 6 electronic mass flow controllers. Fully Automated Analysis The instrument is operated using IGCWin PC software allowing the selection of up to 10 different probe molecules in one experiment and the consecutive analyses of 2 separate columns. providing access to many important physicochemical properties of materials. Quick and Easy Sample Preparation The use of straight 300mm glass columns with the unique SMS column packer means that a typical sample can be packed reproducibly in less than 5 minutes. A wide range of experimental possibilities is available in the standard configuration including both pulsed and frontal probe molecule injection. a fixed volume injection loop and isothermal vapour generation means that the SMS IGC provides an experimental reproducibility never before possible with conventional GC injection systems. Controlled Release Polymers Phase Transition Temperatures e.g.g. Surface Chemistry Dispersive Surface Energy e.g.g. Comprehensive data analysis software brings the results to your desktop with a few clicks of a mouse. Filtration Characteristics of Activated Carbons Acid-Base Properties e.g.g. Stability of Drug Polymorphs FL A VO URINGS N A D PE RFU MES M E IN R L A S A M R A C EU TICA LS FI BR ES . Amorphous recrystallisation in Pharmaceuticals Solubility Parameters e. Persistence of Perfumes on Cotton PH Bulk Properties Diffusion Coefficients e.g. iG C S O R P T I O N S O L U T I O N S The SMS iGC has been designed as a powerful research and QA tool. and the independent control of humidity (%RH) in the carrier gas stream.
in particular those with some degree of amorphous character. The observed lowering of the Tg with increasing %RH can have a dramatic impact upon the storage and processing stability of polymeric materials. This information can be used to explain the differences in surface chemistry and therefore dissolution behaviour of the different batches. Surface heterogeneity can have a significant impact upon the performance and handling of particulate solids.4 Dioxane and Ethyl Acetate on batch A indicates an increased availability of hydrophilic acidic sites on the surface. even though the highest energy sites remain unchanged. Variation of the Tg of Maltose as a function of %RH . CASE STUDY 3: HUMIDITY DEPENDENCE OF GLASS TRANSITION TEMPERATURE As well as surface properties IGC may also be used to measure properties of the bulk material such as glass transition temperatures. In this case the much higher specific free energies measured for 1.CASE STUDY 1: BATCH-TO-BATCH VARIABILITY IGC may be used to determine batch-to-batch variations in surface chemistry which may impact upon the processing or final performance of a material. the processing of the material is shown to modify the surface chemistry and hence the observed dissolution rates. Specific interactions on three batches of a pure drug measured by IGC CASE STUDY 2: SURFACE HETEROGENEITY IN BINARY MIXTURES IGC may also be used to determine the surface heterogeneity (distribution of surface sites) of single phases or multicomponent mixtures. In this case the variation in glass transition temperature (Tg) with relative humidity (%RH) has been measured by IGC for the complex sugar maltose. Batch A gave a good dissolution profile whereas batch C did not and batch B was just outside the accepted tolerance. In this example IGC was successfully used to correlate differences in specific polar interactions for three batches of a pure drug material with their corresponding dissolution rates. In this case. magnesium stearate and a 98%:2% mixture of the example. In this case IGC was used to determine the heterogeneity profiles of lactose monohydrate. The data shows that by adding 2% by weight of magnesium stearate the distribution of surface sites available for interaction is significantly altered. These results may be correlated with process properties such as powder handling or performance properties such as aerosol dispersion for Surface heterogeneity profiles for lactose. magnesium stearate and a 98%:2% mixture of the two materials.
iG C C O N T R O L S O F T W A R E Easy to Learn and Use Realtime Display Of Experiment Progress Quick-set Methods Save and Restore Methods Batch Running of up to 10 Methods Preconditioning Methods Wide Range of Method Variables. Flow Rate and Probe Molecule Concentration User Programmable Probe Molecule Database iG C A N A L Y S I S S O F T W A R E Quick and Easy Data Plotting Raw Data Analysis Dead-Time Correction Surface Energy Heat of Sorption Isotherm Plotting %RH / Flow Rate Plot Performance Test Elutant Properties Database Example plots generated using the IGC analysis software running under Microsoft Excel . Probe Molecule. Temperature. %RH.
Instrument Reproducibility Specific component of surface energy <3% standard deviation.uk www.com www.95 p/pº (dependent upon probe molecules used) Customised Column Oven on request Standard Detectors Thermal Conductivity (TCD) and Flame Ionisation (FID) in series.com SURFACE MEASUREMENT SYSTEMS s m s Design: Kingfisher Design • Photography: Michael Owen • Illustrations: Andrew Green . A below for 12 consecutive measurements on the same column packed with paracetamol) Column-to-Column Reproducibility Specific component of surface energy <4% standard deviation. Suite D Allentown. Temperature range ambient+5°C – 50°C (dependent upon probe molecules used) Probe Molecule Injection Fixed volume injection loop with electronic mass flow controllers.* (See Fig. B below for single measurements on 22 different columns packed with paracetamol) * For a homogeneous material Fig. NA 2222 South 12th Street. Temperature range 5°C – 120°C with 0.02 – 0. PA 18103 Tel: (610) 798 8299 Fax: (610) 798 0334 email: firstname.lastname@example.org USA and CANADA Surface Measurement Systems.co. Internal diameters 2mm.smsuk. Warple Way London W3 0RF Tel: +44 (0)20 8749 4900 Fax: +44 (0)20 8749 6749 email: igc@smsuk. 3mm and 4mm Probe Molecule Oven Forced air circulation type.smsna.1°C stability Sample Columns 300mm x 6mm o.d. (See Fig.S M S iG C I N S T R U M E N T S P E C I F I C A T I O N S Standard Column Oven Dual column aluminium block with thermoelectric heating and sub-ambient cooling.co. dimethyldichlorosilane treated glass. A SMS iGC Instrument Reproducibility Fig. Concentration range 0. B SMS iGC Column-to-Column Reproducibility For more information on any of the following please contact us: iGC Sample Analysis iGC Literature Database iGC Application Notes iGC Product Demonstration SMS Seminars and Workshops DVS – Dynamic Vapour Sorption VGI – Vapour Generator Instrument Confidential Consultancy WORLDWIDE Surface Measurement Systems Ltd 3 Warple Mews.
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