Gas AdsorptionUltra-micropore analysis (< 1.0 nm)Micropore analysis (< 2.0 nm)Mesopore analysis (2 – 50 nm)Pore volume measurementPore size distribution measurement Specific surface area (BET) measurementSpecific probe gases availableMercury PorosimetryMercury intrusion and extrusion optionsMesopore & Macropore analysis (3.5 nm – 650 µm)Pore volume measurementPore size distribution measurementAbsolute porosity, bulk density and skeletal densityPermeability and tortuosity measurementCavity to throat size measurementHelium PycnometryAbsolute density measurementChemisorption and Temperature Programmed AnalysisApplication to active metal doped mediaActive component dispersion and surface areaReduction, oxidation and desorption temperature profiles
Key Analytical Techniques
Ceramicsandfiltermediaareappliedtoaverybroadrangeofapplicationsandareintendedforexposuretoa diverserangeofoperatingconditionsandinteractingspecies.Requirementsofporesize,porevolumeand specificsurfaceareathereforecoverawiderangeareusuallyverydemandingwithrespecttotheabsolute values.AtMCAServicesweofferacompletesuiteofanalyticaltechniqueswhichallowsforthecomplete characterisationofporositythroughouttherangesofmicropores(<2nmdiameter)throughtomacro-pores (upto650µm).Whentheceramicorfiltermediaisdopedwithachemicallyactivemetalliccomponent, chemisorptionoptionsbecomeparticularlyuseful.Chemisorptionprovidesthemeansofanalysingtheactive component alone for its surface area, crystallite size and, importantly, chemical availability via its dispersion.
Determination of pore size and volumeDetermination of absolute porositySelection and control of raw material constituentsFormulation and fabrication process control Identification of optimum fabrication conditionsSelection of materials for specific applicationsMonitoring of products for efficacy during useInvestigation product failure and performance issuesInvestigating product regenerationApplication to filtration of gaseous environmentsApplication to fluid environments and water treatment
Key Applications
Theporosityofceramicsandfiltermediaisofteninextricablylinkedtotheirperformanceinawiderangeof applications.Whenselecting,assessingorproducingceramicsandfiltermediaitisnecessarytoconsiderthe requiredporouscharacteristicswithrespecttotheintendedapplication.Changesinporosityalsoneedtobe consideredduringproductuse,especiallywithregardtocapacitythresholds,poreblockingorfoulingand productregeneration.Theporousnatureofrawmaterialpowders,togetherwithmanufacturingconditions, often dictate the ultimate pore size and volume of a finished product, and therefore its efficacy.
CERAMICS & FILTER MEDIA
BET Surface Area - including krypton adsorption for low area materialsMercury Intrusion Porosimetry - pore size, pore volume & pore area distributionMercury Extrusion Porosimetry - for cavity to throat size evaluationPermeability and Tortuosity measurement via Mercury Porosimetry Gas Adsorption - pore size, area and volume distribution in the micropore and mesopore rangesDensity measurement - absolute density, bulk density, skeletal density & particle densitySpecific probe gases, e.g. H2, CO2, O2 etc available for adsorption capacity measurement
Key Analytical Techniques
Porous charaterisation of geological samplesPorous charatcerisation of construction materialsPorosity characterisation for fluid flow and retentionPorosity characterisation for gas storage and retentionInteraction with specific gases: hydrogen and CO2Assessment of ageing, disintegration and life-cycle Product development: constituents and blendsProduct application and surface treatments
Key Applications
Understandingtheporouscharacteristicsofsolidmaterialsisoftenofcriticalimportancethroughout geologicalandconstructionindustriesanddisciplines.Porositydirectlydeterminesthebehaviour betweenamaterialandafluidmedia:thisincludesfluidflowthroughasample,fluidretention,dryingand curing properties, degradation characteristics and adhesion properties. Theporosityofgeologicalmaterialsisofgreatimportanceacrossdisciplinesofhydro-geology,petrology, environmentalengineeringandgeo-chemistry.Poresizescanvaryenormously:largerporeshavea greaterinteractionwithfluidmediawhilstsmallerporesareofparticularimportancetogaseous permittivity,retentionandstorage.Understandingporositywithinsmallporesis,therefore,ofcritical importancetosectorsconcernedwithbothconventionalandun-conventionalenergyandnet-zero technologies. Theinteractionoffluidswithconstructionmaterialsissignificantthroughouttheirlife-cycle,fromdrying andcuringcharacteristicsofconcretesandcoatingstothroughtheagingprocess-ultimatelyinfluencing theirlife-timeanddegradationcharacteristics.Theporosityoftheconstituentpowdermaterialsorpowder blendheavilyinfluencestheusageandperformancecharacteristicsofthematerials,forexampledrying times, shelf life and adhesion qualities.
CONSTRUCTION & GEOLOGY
MCA Services offers a complete suite of techniques for the physical characterisation of catalyst systems. The combination of mercury porosimetry and gas adsorption provides characterisation throughout the pore size range, from micropores through to macro-pores with a maximum size of ~ 650 µm. Mercury porosimetry can be extended to consider extrusion analysis for consideration of pore geometry and also permeability and tortuosity determination. Most gas adsorption options also include the calculation of BET surface area as standard. Whilst nitrogen adsorption is the most commonly applied technique, alternatives are available for more specialised analyses. For example carbon dioxide for ultra-micropores with the capability of combination with nitrogen adsorption to complete a single, harmonious, pore size distribution. Argon adsorption is available for micro-porous materials proving problematic for nitrogen adsorption, for example those with charged surface species such as zeolites and organic frameworks. Chemisorption (chemical adsorption) is routinely applied to the analysis of active metal constituents to determine their availability for a desired catalytic reaction. Active metal dispersion, surface area and crystallite size are commonly applied and at MCA Services we offer dynamic (pulse) chemisorption using hydrogen and carbon monoxide probe molecules. We also offer more specialised options, for example nitrous oxide and ammonia to ensure that the majority of active metals and loadings can be analysed with confidence. Alongside chemisorption, our Temperature Programmed options provide analyses for reduction, oxidation and desorption, completing the characterisation and understanding of active constituents.
Gas Adsorption: pore size, area and volume determination in the micropore and mesopore ranges.Gas Adsorption: BET Surface Area.Mercury Porosimetry: pore size, area and volume determination in meso & macropore ranges.Mercury Intrusion / Extrusion Porosimetry: cavity to throat size determination. Permeability and Tortuosity: measurement by mercury intrusion porosimetry.Chemisorption: active metal surface area and dispersion measurement – static and dynamic methods.Temperature Programmed Methods: reduction, oxidation, adsorption & desorption. Density Measurement: absolute density, bulk (envelope) density and skeletal density
Traditionalporositycharacterisationtechniques,suchasnitrogengasadsorptionandmercuryporosimetry canbeappliedtovirtuallyanysolidform,frompowderstogranulesandextrudates.Theporousnatureof thematerialcanthusbeexplored,frommicroporesthroughtolargerinter-particulateorinter-granular pores(theclassictransportpores).However,duetophysicalandphysico-chemicalpropertiesofthe adsorbent,specificadsorbatesoftenrequirededicatedanalyses.Wethereforeofferacomprehensive rangeofadsorbateoptions,notablyhydrogenandcarbondioxidewhichcanbeappliedtogasadsorption andtemperatureprogrammedanalysesinordertodeterminethesorptionabilityandcapacityundermore specific conditions.
BET Surface Area: rapid porosity assessmentGas adsorption: micro- and meso-pore characterisationGas adsorption: sorption capacityGas adsorption: heat of adsorptionGas adsorption: N2, H2 and CO2 optionsMercury porosimetry: meso and macro-pore characterisationMercury porosimetry: absolute porosityMercury porosimetry: permeability and tortuosityTemperature programmed desorption: sorption capacity and kinetics
Key Techniques
Themovetowardsgreener,environmentallyfriendlytechnologiesplacesincreasingdemandsonthe identification,developmentandfabricationofmaterialshavingpreciselycontrolledphysicalandphysico-chemicalproperties.Essentiallymaterialsmustadsorbandretainadesiredspecies,withthepotentialto laterreleasethespeciesunderspecificconditionsdependingontheapplication.Physicalmaterial propertiesarecentraltothedevelopmentofgreenmaterials.Characteristicsofporosity,suchaspore volume,poresizeandporegeometrydeterminethesorptionprocess:whetheraspeciescanadsorbtothe materialreasonablyeasily,whetheritwillberetained,theeaseofitsremovalandcritically,thequantity whichmaybeadsorbed.Physico-chemicalproperties,notablythepresenceandextentofchargedsurface speciesalsoplayacriticalroleintheadsorptionprocessandmaybebeneficialordetrimentaldepending on the nature of a particular adsorbate.
CARBON CAPTURE AND HYDROGEN STORAGE
PoresizespresentwithinelectrodestypicallyfallwithintherangeanalysedbytheMercuryPorosimetry technique.Thiscanbeextendedtoconsiderpermeability,ausefulcomparisontoolwhenconsideringfluid flowintoandthroughaporoussample.Thistechniqueisalsoapplicabletotheanalysisofseparator materials where a tight distribution of pore sizes is often demanded for efficient transport.
Determination of separator pore size and porosityOptimisation of slurry compositionOptimisation of calendaring processOptimisation of drying processCharacterisation of anode porosityCharacterisation of cathode porosityDirect relationships with electrode performanceEfficiency and capacityCharge & Discharge performanceCycle lifetimeCharging characteristicsElectrolyte transport
Assessment of porous nature of raw materials for formulationQuality control of incoming raw materialsSurface area and porosity of high area carbons & graphitesSurface area and porosity of active cathode materialCharacterisation of inter-particulate porosityFormulation of binder composition and loadingMeasurement of absolute, bulk and particle densityDetermination of processing conditions
Key Applications - Materials
Theporousnatureofbatterycomponents:anode,cathode,separatorandsolidelectrolyteandalso finishedelectrodearchitectureiscriticaltothedevelopment,performanceandoptimizationofbattery systems. Porouscharacteristicsprofoundlyinfluencetheperformanceofthefinishedcellsincecombinationofthe porousnatureoftherawmaterialsandfabricationstepsapplieddeterminetheultimateporositywithin componentsofthecell.Theporouscharacteristicsoffinishedelectrodesarepartiallydeterminedbythe inter-particulateporosityoftherawmaterials,porositywithinrawmaterialparticles,bindermaterialand loadingandproductionconditionssuchascalendaringanddrying.Electrodeporosityiscriticalinthe determinationofconductivity,energydensity,chargingefficiency,electrolytetransportcharacteristics, cyclinglifetime,availabilityofelectrochemicallyactivesitesandelectrodedegradation.Understanding porosityallowsforfocusedselectionofrawmaterialsandoptimisationofprocessingconditions.Complete understandingoftheporouscharacterofmaterialsis,therefore,criticaltoallstagesofmaterials selection, cell development and electrode processing.
BATTERY TECHNOLOGY
Mercury PorosimetryPore volume DistributionPore Size DistributionPore Area DistributionAbsolute PorosityBulk and Skeletal DensityPore GeometryPermeability MeasurementApplicable to all solid formsGas AdsorptionBET Specific Surface Area by NitrogenBET Specific Surface Area by Krypton (low SSA)Micro-pore / Meso-pore characterisationPore volume DistributionPore Size DistributionPore Area Distribution
Key Analytical Techniques
Characterisation of API and excipient materialsCharacterisation of powder blendsInvestigation of batch failures and inter-batch variabilityInfluence of stability trials on porosityDetermination of long-term stability and shelf lifeInvestigation and establishment of tabletting conditions Identification of counterfeit batchesSignificant to approval processesAll analyses undertaken to ISO 17025 standards
Key Applications
Thephysicalcharacteristicsofpharmaceuticalsprofoundlyinfluencethepropertiesandeffectivenessof thefinaldosageform,beitadministeredviatablet,granule/capsuleorinhalationroutes.Furthermore, knowledgeofphysicalcharacteristicsoftencontributestothecriticalunderstandingofallcomponents, suchasAPI,excipients,powderblendsandintermediateribbonsaswellasthefinalform.Thisisapplicable toallstagesofpharmaceuticalprocesses:fromformulationthroughmanufacturingtoqualitycontrol, stability trials and trouble-shooting atypical behaviour. Physicalcharacteristicscommonlyincludespecificsurfacearea(SSA),poresizedistribution,porevolume anddensity,whichtogetherprovideacompleteunderstandingofporouscharacter.Inturn,porosityhas directeffectsonmanyaspectsofperformance,forexampledissolutionanddisintegrationrates,strength andhardnessandlongtermstability.Theyalsoinfluenceformulationandeffectstabilityofsolid components in many emulsion, paste and topical forms. Porosityinpharmaceuticalmaterialscanbepresentinvariouslocations:withintabletcoresandgranules, coatings,withintheparticlesofapre-cursorpowderblendandalsothevoidspacesbetweenpowder particles.Thelatterdictatestheporouscharacteristicsoftablettedforms.SSAmeasurementisroutinely andusefullyappliedtothecharacterisationofpowdersamplesbuttheporesizespresentcommonlyfall withintherangemeasuredbythemercuryporosimetrytechnique,inwhichSSAmeasurementsareless sensitive.Porosimetrythusprovidesacompletepictureofporesize,porevolume,absoluteporosityand density,aswellasprovidinginsighttoporegeometry.Theseporositycharacteristics,whichdictate performancebehaviours,maybeindicativeofatypicalperformance,andoftenchangeduringtheaging processes applied during stability trials. AtMCAServicesweofferasuiteofanalyticaltechniquesforthecompletecharacterisationof pharmaceuticalsamples.Thisiscombinedwiththeexperienceandexpertisetoactivelyassistwiththe interpretationofresultsdirectlyrelatingthesetoperformancecharacteristicsofthematerial.Wehave manyyearsofexperiencepartneringwiththepharmaceuticalsector,consideringawidevarietyofdosage formsandapplications,fromformulationtostabilitytrialsandidentificationoftheinfluenceofporosityto materials and batches having atypical behaviour.
Product development and formulationDetermination of product specificationsDetermination of stability and shelf lifeControl and assessment of raw materialsGeneration of Quality Control dataAnalysis of performance loss during useMaterial regenerationDetermination of consistencyIdentification of factors influencing performanceInvestigations into product failureEconomising material usageDetermination of the effects of additivesDevelopment of process control Provision of critical QbD framework dataLitigation support and patent formulation
Key Applications
AdsorbentsAlumina and SilicaCarbons, Charcoals and GraphitesCatalystsCeramicsCoatingsFilms, Fabrics and MembranesMetal Organic FrameworksMetallic Compounds and OxidesPharmaceutical Tablets and PowdersPolymersZeolites
Materials
TheanalyticaltestsofferedbyMCAServicesprovideawealthofinformationdescribingthephysicaland physico-chemicalnatureofmaterials,includingporouscharacteristicsandchemicalactivity.Such informationisinvaluabletomanysectorsandapplications,forexample:aspartofroutinequalitycontrol, rawmaterialassessment,researchanddevelopmentandproductfailureinvestigations.Someexamples ofsectorsandapplicationsthathavebenefitedfromouranalyticaltechniquesandinsightarehighlighted below.Theporouscharacteristicsofmaterialsoftenhaveprofoundeffectsonefficacyandperformance.Porosity maybedescribedbyacombinationoffeatures:specificsurfacearea,porevolume,poresizedistribution, poregeometry,particlesizeandgeometryandsampledensity.Theseareoftenconsideredincombination toobtainacompletedescriptionofporosityandcanbeappliedtovirtuallyanysolidform,fromfine particulate matter through to larger solid forms.
Product development and formulationDetermination of product specificationsDetermination of stability and shelf lifeControl and assessment of raw materialsGeneration of Quality Control dataAnalysis of performance loss during useMaterial regeneration
Key Applications
AdsorbentsAlumina and SilicaCarbons, Charcoals and GraphitesCatalystsCeramicsCoatings
Materials
TheanalyticaltestsofferedbyMCAServicesprovideawealthof informationdescribingthephysicalandphysico-chemicalnatureof materials,includingporouscharacteristicsandchemicalactivity.Such informationisinvaluabletomanysectorsandapplications,forexample: aspartofroutinequalitycontrol,rawmaterialassessment,research anddevelopmentandproductfailureinvestigations.Someexamplesof sectorsandapplicationsthathavebenefitedfromouranalytical techniques and insight are highlighted below.Theporouscharacteristicsofmaterialsoftenhaveprofoundeffectson efficacyandperformance.Porositymaybedescribedbyacombination offeatures:specificsurfacearea,porevolume,poresizedistribution, poregeometry,particlesizeandgeometryandsampledensity.These areoftenconsideredincombinationtoobtainacompletedescriptionof porosityandcanbeappliedtovirtuallyanysolidform,fromfine particulate matter through to larger solid forms.
Films, Fabrics and MembranesMetal Organic FrameworksMetallic Compounds and OxidesPharmaceutical Tablets and PowdersPolymersZeolites
Determination of consistencyIdentification of factors influencing performanceInvestigations into product failureEconomising material usageDetermination of the effects of additivesDevelopment of process control Provision of critical QbD frameworkdataLitigation support and patent formulation
Gas AdsorptionUltra-micropore analysis (< 1.0 nm)Micropore analysis (< 2.0 nm)Mesopore analysis (2 – 50 nm)Pore volume measurementPore size distribution measurement Specific surface area (BET) measurementSpecific probe gases availableMercury PorosimetryMercury intrusion and extrusion optionsMesopore & Macropore analysis (3.5 nm – 650 µm)Pore volume measurementPore size distribution measurementAbsolute porosity, bulk density and skeletal densityPermeability and tortuosity measurementCavity to throat size measurementHelium PycnometryAbsolute density measurementChemisorption and Temperature Programmed AnalysisApplication to active metal doped mediaActive component dispersion and surface areaReduction, oxidation and desorption temperature profiles
Key Analytical Techniques
Ceramicsandfiltermediaareappliedtoaverybroadrangeof applicationsandareintendedforexposuretoadiverserangeof operatingconditionsandinteractingspecies.Requirementsofpore size,porevolumeandspecificsurfaceareathereforecoverawide rangeareusuallyverydemandingwithrespecttotheabsolutevalues. AtMCAServicesweofferacompletesuiteofanalyticaltechniques whichallowsforthecompletecharacterisationofporositythroughout therangesofmicropores(<2nmdiameter)throughtomacro-pores(up to650µm).Whentheceramicorfiltermediaisdopedwithachemically activemetalliccomponent,chemisorptionoptionsbecomeparticularly useful.Chemisorptionprovidesthemeansofanalysingtheactive componentaloneforitssurfacearea,crystallitesizeand,importantly, chemical availability via its dispersion.
Determination of pore size and volumeDetermination of absolute porositySelection and control of raw material constituentsFormulation and fabrication process control Identification of optimum fabrication conditionsSelection of materials for specific applicationsMonitoring of products for efficacy during useInvestigation product failure and performance issuesInvestigating product regenerationApplication to filtration of gaseous environmentsApplication to fluid environments and water treatment
BET Surface Area - including krypton adsorption for low area materialsMercury Intrusion Porosimetry - pore size, pore volume & pore area distributionMercury Extrusion Porosimetry - for cavity to throat size evaluationPermeability and Tortuosity measurement via Mercury Porosimetry Gas Adsorption - pore size, area and volume distribution in the micropore and mesopore rangesDensity measurement - absolute density, bulk density, skeletal density & particle densitySpecific probe gases, e.g. H2, CO2, O2 etc available for adsorption capacity measurement
Key Analytical Techniques
Porous charaterisation of geological samplesPorous charatcerisation of construction materialsPorosity characterisation for fluid flow and retentionPorosity characterisation for gas storage and retentionInteraction with specific gases: hydrogen and CO2Assessment of ageing, disintegration and life-cycle Product development: constituents and blendsProduct application and surface treatments
Key Applications
Understandingtheporouscharacteristicsofsolidmaterialsisoftenof criticalimportancethroughoutgeologicalandconstructionindustries anddisciplines.Porositydirectlydeterminesthebehaviourbetweena materialandafluidmedia:thisincludesfluidflowthroughasample, fluidretention,dryingandcuringproperties,degradation characteristics and adhesion properties. Theporosityofgeologicalmaterialsisofgreatimportanceacross disciplinesofhydro-geology,petrology,environmentalengineeringand geo-chemistry.Poresizescanvaryenormously:largerporeshavea greaterinteractionwithfluidmediawhilstsmallerporesareof particularimportancetogaseouspermittivity,retentionandstorage. Understandingporositywithinsmallporesis,therefore,ofcritical importancetosectorsconcernedwithbothconventionalandun-conventional energy and net-zero technologies. Theinteractionoffluidswithconstructionmaterialsissignificant throughouttheirlife-cycle,fromdryingandcuringcharacteristicsof concretesandcoatingstothroughtheagingprocess-ultimately influencingtheirlife-timeanddegradationcharacteristics.Theporosity oftheconstituentpowdermaterialsorpowderblendheavilyinfluences theusageandperformancecharacteristicsofthematerials,for example drying times, shelf life and adhesion qualities.
MCA Services offers a complete suite of techniques for the physical characterisation of catalyst systems. The combination of mercury porosimetry and gas adsorption provides characterisation throughout the pore size range, from micropores through to macro-pores with a maximum size of ~ 650 µm. Mercury porosimetry can be extended to consider extrusion analysis for consideration of pore geometry and also permeability and tortuosity determination. Most gas adsorption options also include the calculation of BET surface area as standard. Whilst nitrogen adsorption is the most commonly applied technique, alternatives are available for more specialised analyses. For example carbon dioxide for ultra-micropores with the capability of combination with nitrogen adsorption to complete a single, harmonious, pore size distribution. Argon adsorption is available for micro-porous materials proving problematic for nitrogen adsorption, for example those with charged surface species such as zeolites and organic frameworks. Chemisorption (chemical adsorption) is routinely applied to the analysis of active metal constituents to determine their availability for a desired catalytic reaction. Active metal dispersion, surface area and crystallite size are commonly applied and at MCA Services we offer dynamic (pulse) chemisorption using hydrogen and carbon monoxide probe molecules. We also offer more specialised options, for example nitrous oxide and ammonia to ensure that the majority of active metals and loadings can be analysed with confidence. Alongside chemisorption, our Temperature Programmed options provide analyses for reduction, oxidation and desorption, completing the characterisation and understanding of active constituents.
Gas Adsorption: pore size, area and volume determination in the micropore and mesopore ranges.Gas Adsorption: BET Surface Area.Mercury Porosimetry: pore size, area and volume determination in meso & macropore ranges.Mercury Intrusion / Extrusion Porosimetry: cavity to throat size determination. Permeability and Tortuosity: measurement by mercury intrusion porosimetry.Chemisorption: active metal surface area and dispersion measurement – static and dynamic methods.Temperature Programmed Methods: reduction, oxidation, adsorption & desorption. Density Measurement: absolute density, bulk (envelope) density and skeletal density
Key Techniques
Thesignificanceandinfluenceoftheporousnatureofcatalystsystems withrespecttotheirfunctionality,performanceandefficiencyiswell known,asistheunderstandingofthephysico-chemicalpropertiesof theactiveconstituents.Characterisationoftheporousnatureof catalystscanbeappliedtotheactiveconstituents,supportmaterialsor thefinishedsystem.Understandingtheporousandactivenatureof catalystsisvitaltobothun-usedandspentmaterialsandalsowhen considering degradation and the regeneration process.
Traditionalporositycharacterisationtechniques,suchasnitrogengas adsorptionandmercuryporosimetrycanbeappliedtovirtuallyany solidform,frompowderstogranulesandextrudates.Theporousnature ofthematerialcanthusbeexplored,frommicroporesthroughtolarger inter-particulateorinter-granularpores(theclassictransportpores). However,duetophysicalandphysico-chemicalpropertiesofthe adsorbent,specificadsorbatesoftenrequirededicatedanalyses.We thereforeofferacomprehensiverangeofadsorbateoptions,notably hydrogenandcarbondioxidewhichcanbeappliedtogasadsorption andtemperatureprogrammedanalysesinordertodeterminethe sorption ability and capacity under more specific conditions.
BET Surface Area: rapid porosity assessmentGas adsorption: micro- and meso-pore characterisationGas adsorption: sorption capacityGas adsorption: heat of adsorptionGas adsorption: N2, H2 and CO2 optionsMercury porosimetry: meso and macro-pore characterisationMercury porosimetry: absolute porosityMercury porosimetry: permeability and tortuosityTemperature programmed desorption: sorption capacity and kinetics
Key Techniques
Themovetowardsgreener,environmentallyfriendlytechnologies placesincreasingdemandsontheidentification,developmentand fabricationofmaterialshavingpreciselycontrolledphysicaland physico-chemicalproperties.Essentiallymaterialsmustadsorband retainadesiredspecies,withthepotentialtolaterreleasethespecies underspecificconditionsdependingontheapplication.Physical materialpropertiesarecentraltothedevelopmentofgreenmaterials. Characteristicsofporosity,suchasporevolume,poresizeandpore geometrydeterminethesorptionprocess:whetheraspeciescan adsorbtothematerialreasonablyeasily,whetheritwillberetained, theeaseofitsremovalandcritically,thequantitywhichmaybe adsorbed.Physico-chemicalproperties,notablythepresenceand extentofchargedsurfacespeciesalsoplayacriticalroleinthe adsorptionprocessandmaybebeneficialordetrimentaldependingon the nature of a particular adsorbate.
Poresizespresentwithinelectrodestypicallyfallwithintherange analysedbytheMercuryPorosimetrytechnique.Thiscanbeextended toconsiderpermeability,ausefulcomparisontoolwhenconsidering fluidflowintoandthroughaporoussample.Thistechniqueisalso applicabletotheanalysisofseparatormaterialswhereatight distribution of pore sizes is often demanded for efficient transport.
Determination of separator pore size and porosityOptimisation of slurry compositionOptimisation of calendaring processOptimisation of drying processCharacterisation of anode porosityCharacterisation of cathode porosityDirect relationships with electrode performanceEfficiency and capacityCharge & Discharge performanceCycle lifetimeCharging characteristicsElectrolyte transport
Key Applications - Components
Understandingparticleporosityisvitaltotheselectionandcontrolof highsurfaceareacomponents,suchascarbonsandgraphites,aswell asmonitoringcathodematerialsandassessingtheintercalation procedure.Fullcharacterisationofinter-particulateporosityis essentialasthisdescribespackingcharacteristicswhich,in combinationwithprocessingconditions,determinetheporosityofthe finishedelectrodeThisinvolvesfullyunderstandinginter-particulate spaces beyond that suggested by particle size alone.
Assessment of porous nature of raw materials for formulationQuality control of incoming raw materialsSurface area and porosity of high area carbons & graphitesSurface area and porosity of active cathode materialCharacterisation of inter-particulate porosityFormulation of binder composition and loadingMeasurement of absolute, bulk and particle densityDetermination of processing conditions
Key Applications - Materials
Theporousnatureofbatterycomponents:anode,cathode,separator andsolidelectrolyteandalsofinishedelectrodearchitectureiscritical to the development, performance and optimization of battery systems. Porouscharacteristicsprofoundlyinfluencetheperformanceofthe finishedcellsincecombinationoftheporousnatureoftheraw materialsandfabricationstepsapplieddeterminetheultimate porositywithincomponentsofthecell.Theporouscharacteristicsof finishedelectrodesarepartiallydeterminedbytheinter-particulate porosityoftherawmaterials,porositywithinrawmaterialparticles, bindermaterialandloadingandproductionconditionssuchas calendaringanddrying.Electrodeporosityiscriticalinthe determinationofconductivity,energydensity,chargingefficiency, electrolytetransportcharacteristics,cyclinglifetime,availabilityof electrochemicallyactivesitesandelectrodedegradation. Understandingporosityallowsforfocusedselectionofrawmaterials andoptimisationofprocessingconditions.Completeunderstandingof theporouscharacterofmaterialsis,therefore,criticaltoallstagesof materials selection, cell development and electrode processing.
Mercury PorosimetryPore volume DistributionPore Size DistributionPore Area DistributionAbsolute PorosityBulk and Skeletal DensityPore GeometryPermeability MeasurementApplicable to all solid formsGas Adsorption
Key Analytical Techniques
Characterisation of API and excipient materialsCharacterisation of powder blendsInvestigation of batch failures and inter-batch variabilityInfluence of stability trials on porosityDetermination of long-term stability and shelf lifeInvestigation and establishment of tabletting conditions Identification of counterfeit batchesSignificant to approval processesAll analyses undertaken to ISO 17025 standards
Key Applications
Thephysicalcharacteristicsofpharmaceuticalsprofoundlyinfluence thepropertiesandeffectivenessofthefinaldosageform,beit administeredviatablet,granule/capsuleorinhalationroutes. Furthermore,knowledgeofphysicalcharacteristicsoftencontributesto thecriticalunderstandingofallcomponents,suchasAPI,excipients, powderblendsandintermediateribbonsaswellasthefinalform.This isapplicabletoallstagesofpharmaceuticalprocesses:from formulationthroughmanufacturingtoqualitycontrol,stabilitytrials and trouble-shooting atypical behaviour. Physicalcharacteristicscommonlyincludespecificsurfacearea(SSA), poresizedistribution,porevolumeanddensity,whichtogetherprovide acompleteunderstandingofporouscharacter.Inturn,porosityhas directeffectsonmanyaspectsofperformance,forexampledissolution anddisintegrationrates,strengthandhardnessandlongtermstability. Theyalsoinfluenceformulationandeffectstabilityofsolidcomponents in many emulsion, paste and topical forms. Porosityinpharmaceuticalmaterialscanbepresentinvarious locations:withintabletcoresandgranules,coatings,withinthe particlesofapre-cursorpowderblendandalsothevoidspaces betweenpowderparticles.Thelatterdictatestheporous characteristicsoftablettedforms.SSAmeasurementisroutinelyand usefullyappliedtothecharacterisationofpowdersamplesbutthepore sizespresentcommonlyfallwithintherangemeasuredbythemercury porosimetrytechnique,inwhichSSAmeasurementsarelesssensitive. Porosimetrythusprovidesacompletepictureofporesize,porevolume, absoluteporosityanddensity,aswellasprovidinginsighttopore geometry.Theseporositycharacteristics,whichdictateperformance behaviours,maybeindicativeofatypicalperformance,andoften change during the aging processes applied during stability trials. AtMCAServicesweofferasuiteofanalyticaltechniquesforthe completecharacterisationofpharmaceuticalsamples.Thisiscombined withtheexperienceandexpertisetoactivelyassistwiththe interpretationofresultsdirectlyrelatingthesetoperformance characteristicsofthematerial.Wehavemanyyearsofexperience partneringwiththepharmaceuticalsector,consideringawidevariety ofdosageformsandapplications,fromformulationtostabilitytrials andidentificationoftheinfluenceofporositytomaterialsandbatches having atypical behaviour.
BET Specific Surface Area by NitrogenBET Specific Surface Area by Krypton (low SSA)Micro-pore / Meso-pore characterisationPore volume DistributionPore Size DistributionPore Area Distribution