Investigation of relationship between solid sample and fluid mediaPassage and retention capabilities of fluids and gases in solid materials:
Key Applications
Geological and geo-technical testingPetrology and HydrologyBattery electrodes: electrolyte flow and active site accessibilityBattery separators: electrolyte flow propertiesCatalyst testing: accessibility to active sitesPharmaceuticals: dissolution and disintegration propertiesFilter media: flow and retention propertiesMembranes and papers: flow throughout propertiesCeramics: flow throughput and capacity properties
Sample permeability and tortuosity measurement is offered as an extension to our standard mercury porosimetry analysis options, obtaining porosity and permeability information in a single analysis which provides a wealth of information in a short time-frame. Permeability is a measure of fluid or gas flow through a porous solid sample. It is, therefore, of considerable interest in applications where a solid material interacts with a liquid or gas. Permeability measurement from mercury intrusion analysis was originally developed with regard to geological samples, but it has since found significant application to a wide variety of sample types and sectors. Pore tortuosity, obtained from characteristics of pore size, pore volume, pore area and permeability is a measure of the tortuous pathway of pores through a sample: essentially a representation of how direct the pore pathway is as it passes through a sample. This can be particularly useful when comparing samples.
Pore volume (numerical and graphical reports)Pore Size Distribution (numerical and graphical reports)Pore Area (numerical and graphical reports)Average pore size by numerous calculationsAdditional calculation of bulk and skeletal densityAdditional calculation of absolute porosity (% volume)Characterisation of inter-particulate and intra-particulate porosityPermeability and Tortuosity measurementMercury intrusion and intrusion / extrusion optionsPore geometry assessment and cavity-to-throat size ratioAssessment of particle size via Mayer-Stowe methodExtensive and flexible reporting options
Analysis of wide range of pore sizes 3.5nm to 650 µmApplicable to almost any solid sample formDissolution rate of pharmaceutical tablets and granulesPharmaceutical powder blends and resulting solid dose formsAssessment of powder inter-particulate size and volumeCeramic raw material and finished product characterisationEfficiency and efficacy of filter mediaChemical activity of catalysts and electrocatalystsFabrication of battery electrode, separator and solid electrolytesCapacity and efficiency of battery electrodes and materialsProduction and performance of construction materialsProduction and performance of coatings and abrasivesCharacterisation of geological samples and fluid interactionsProduct life-cycle and capacity assessmentInvestigations of atypical performance and failures
Key Applications
Mercury porosimetry provides a wealth of information for understanding the porous characteristics of any material with porosity in the size range 3.5 nm to 650 µm. The technique is applicable to virtually any solid form, from powders, through granules to single solid pieces, films, membranes, fabrics and coatings. The pore volume, pore area and pore size present in solid materials and between the particles of powder and granules often profoundly affect the fabrication and performance of materials. Porosity influences the efficiency, efficacy and functionality of materials across sectors such as pharmaceuticals, catalysis, energy production and storage, sorption technology and geology & environmental science and construction. It is usually necessary to consider the extent, nature and effects of porosity at all stages of product life-cycle, from the characterisation of raw materials, through formulation and fabrication processes to final use and application. Knowledge of the full porous character of materials is, therefore, critical to the understanding of materials and their application.
MERCURY POROSIMETRY
AtMCAServicessampleanalysisisundertakenusingourMicromeriticsTriStar3030plusand3020 instrument,combinedwithcomprehensivesampledegassingoptionscapableoftemperaturesinthe rangeambientto400°Cunderdynamicvacuumorflowinginertgas.Wecan,therefore,preparevirtually anysamplematerialon-siteimmediatelypriortoanalysis,whichensuresthemostaccurateandreliable measurements are obtained.
Pore volume, area and size distributions – numerically and graphicallyFull gas adsorption and desorption isotherm measurementDetermination of pore geometryBET Specific Surface Area includedAssessment of microporosity via t-plot analysis and DFT / NL-DFTExtensive and flexible analytical and reporting optionsExtensive and flexible sample degassing optionsAvailability of alternative adsorbents: argon and carbon dioxideComprehensive range of data reduction optionsBET Surface AreaBJH Mesopore volume, area and size – adsorption isothermBJH Mesopore volume, area and size – desorption isothermt-plot and α-S plot methodsDFT and NL-DFTLangmuir Surface AreaAssessment of pore geometry from isotherm hysteresisCombination with mercury porosimetry to extend pore size range to 650 µm
Analytical Options and Highlights
Themeasurementofthefullgasadsorptionanddesorptionisothermprovidesafullporosimetryanalysis techniqueforthedeterminationofporevolume,poreareaandporesizeintheporesizerange<2–300nm diameter,togetherwithanassessmentofporegeometry.Nitrogenisanidealadsorbate,providingfull chacterisationthroughoutthemesoporerangeandintothesmallmacroporeregion.CalculationofBET surfaceareaisincludedandtheassessmentoftheextentandvolumeofmicroporositycanalsobe includedthroughspecificallytailoredanalyticalconditions.Formorespecialisedapplicationswealso offer alternative adsorbates such as carbon dioxide adsorption and argon adsorption. Micropores(<2nmdiameter)arecommoninarangeofmaterials,suchascarbonsandnanotubes,zeolites, metalorganicframeworks(MOFs),zeoliticimidazolateframeworks(ZIFs),covalentorganicframeworks (COFs)etc.Microporesarefundamentallyimportanttothefunctionalityandperformanceofmany applications,suchasbatterymaterials,adsorbentsandfilters,catalysts,gasstorageandsequestration materials.Together,microporevolume,areaandsizedirectlyaffectperformancethroughdetermining capacity,accessibility,availabilityofactivesitesandfunctionality.Assessmentofmicroporositycanbe derived from the same adsorption isotherm and included in reported data.
Adsorption capacity and efficacy of adsorbates and filter mediaActivity of catalysts and catalytic processesAssessment of new, spent and regenerated catalysts and filter mediaElectrochemical activity of battery components and constituentsFabrication process development and controlAvailability of biologically available sites in pharmaceuticalsInorganic, alumina and silica precursor and raw material assessmentBehaviour of powder materials for inclusion to pastes and emulsionsRaw material selection and QC processDissolution and dispersion assessment and controlRapid assessment of microporous materials
Key Applications
Theporousnatureofmaterialsaffectsawidevarietyofperformanceaspectsinmanyapplications,suchas adsorptioncapacity,chemicalreactivity,electrochemicalactivity,structuralpropertiesanddissolution rates.Understandingthecomponentsofporosity:porevolume,poresizeandporearea,is,therefore, critical to many sectors and applications. Micropores,mesoporesandsmallmacroporesareconvenientlystudiedbytheanalyticaltechniqueofgas adsorption.Gasadsorptionprovidesporevolume,areaandsizedatainthetypicalporesizerange2–300 nm,althoughtheupperlimitdependsonthenatureofthesample.Considerationofmicroporecontentvia microporevolumeandsurfaceareacanalsobeincludedinasingleanalysis.Thelatest,powerfuland adaptableinstrumentationcombinedwithourdecadesofexperiencemeansthatwecanrecommendthe mostsuitableanalyticaloptionsforyoursamples.Analysesandreportingoptionscanbetailoredto providethemostpertinentinformationtodescribeyourparticularsamplesandspecificapplication.We arealsohappytoassistwithdatainterpretationtoensurethatyouobtainthemostrelevantdataand information.
GAS ADSORPTION POROSIMETRY
Poresizescanbedividedintothreeranges:Micropores(<2nm), Mesopores(2–50nm)andMacropores(>50nm),thesizesrefertothe diameterofacylindricalporeorthewidthofaslit-shapedpore accordingtoIUPACdefinitions.Micro-poresaresometimesfurther dividedtoincludesuper-micropores,orultra-microporeswhichare smallerthan1nm.Poregeometry,whichincludestypesandshapesof pores should also be considered.Thereisnosingletechniquethatcanbeusedtodetermineporous characteristicsthroughouttherangesofporesizes.Therefore,itis usuallynecessarytoselectthemostappropriatetechniqueor combinationoftechniquesforagivensampleandapplication.AtMCA Serviceswehavedecadesofexperienceinthisandarealwayshappyto provide our thoughts on this selection.
Porosimetrycoversarangeofanalyticaltechniquesusedforunderstandingandcharacterisingtheporous natureofmaterials.Porosityoftenhasprofoundaffectsonthebehaviourofmaterialsandinfluencesmany aspects of their selection, fabrication, application, performance and life-cycle. Porosityisabroadtermwhichencompassesphysicalcharacteristicssuchasporevolume,poresurface area,poresizedistribution,specificsurfacearea,absoluteporosityandporegeometry.Italsohasdirect relationshipswiththevariousmeasuresofsampledensity,gasandfluidpermeabilityandchemical activity.AlloftheseaspectsofporositycanbecharacterisedatMCAServicesusingarangeofstate-of-the-artanalyticalinstruments.Ourexpertiseintheapplicationofanalysesandinterpretationmeansthat the most pertinent data is presented and related directly to specific materials and applications. Porosityiscommonlyconsideredasbeingpresentwithinasolidmaterialbutitisalsopresentinthevoid spacesofapowdermaterial.Suchinter-particulateporosityisdeterminedbytheparticlesizeandshapeof thepowdergrains,essentiallyreflectingthepackingpropertiesofpowderparticles.Understandinginter-particulateporositybecomesverysignificantwhenapowderisusedinthefabricationofasolidarticle. Combinedwiththeprocessconditions,suchascompression,bindercompositionandfiringtemperatureit determines the porosity within the finished article.
Forheliumpycnometryanalysis,MCAServiceshasarangeofsamplecellswhichallowfortheaccurate determinationofabsolutedensityusingsamplesquantitiesfrom1cm3to10cm3.Itis,therefore,possibleto analyseawiderangeofsampletypes,fromfinepowderstolargersolidpieces.Ifthetheoreticalabsolute densityofasamplematerialisknownitisalsopossibletocalculatethevolumeofclosedporeswithinthe samplefromtheheliumpycnometryvalue.Suchcalculationisespeciallyusefulwhenconsideringfoam and construction materials as it represents the void volume within the sample material.
Alsotermedtruedensity,excludesthevolumeofall openporeswithinthesampleand,therefore,represents thedensityofjustthesolidmaterial.Thestandard methodusedatMCAServicesisgaspycnometryby heliumdisplacementusingourMicromeriticsAccuPyc instrument.Ifheliumentrapmentisofconcernoptions for using nitrogen are also available.
Temperatureprogrammeddesorptionisusedtostudythe temperaturedependenceandstrengthofinteractionbetweena samplesurfaceandaprobemolecule.Typicalprobemolecules includeH2,CO2andNH3,althoughothers,includingvapours,can alsobeappliedinordertoinvestigatespecificsystems.Initial adsorption,eitherphysicalorchemical,isusuallyconductedat ambienttemperature,althoughsub-ambientconditionscanalso beapplied.Thedesorptionprocessisthenmeasuredwithsteady increasing sample temperature under inert gas flow. Recordingthetemperatureatwhichdesorptionoccursand accuratelymeasuringthevolumeofgasdesorbingallowsforthe determinationofthenumberandstrengthofactiveadsorption sitesonasamplesurface.Temperatureprogrammeddesorption canalsobeextendedtoinvestigatesamplematerialswhenthe adsorption/desorptionprocessesaresignificantto performance,forexampleeffectivenessandregenerationof adsorbents,filtermaterialsandcatalystsandthesorption capacity of storage materials.
Temperature Programmed Desporption (TPD)
Our temperature programmed analyses are part of our suite of chemisorption options, used to investigate reduction, oxidation, desorption and decomposition as a function of temperature. Traditionally these have been applied to the catalysis sector where the understanding of surface reactions are fundamental to the development and regeneration of high efficiency systems. The use of these techniques is now commonly extended to other sectors and applications, particularly hydrogen storage and carbon capture. Temperature programmed analyses at MCA Services are undertaken using our state-of-the-art Micromeritics AutoChem II instrument, capable of analyses from sub-ambient (-70 °C) to 1100 °C. Furthermore, this instrument provides tremendous scope for accurate selection and control over analytical parameters such as gas flow rate, temperature ramp rate and temperature holding ranges. The instrument detector is always calibrated to match specific analytical parameters, ensuring the accurate calculation of active gas consumption.
TEMPERATURE PROGRAMMED ANALYSES
Temperatureprogrammedreductionisusedtoinvestigatethe reducibilityofaspeciesandcanbeappliedtometalsandmetal compoundssuchasoxidesinbothsupportedandun-supported forms.Historicallyveryimportanttothestudyofcatalysts,TPR canbeappliedtoawidevarietyofmetallicandsupported metallicspecieswhenreductionbehaviourrequired understanding.Theanalyticalprocessinvolvesheatingasample atasteadyrate,toamaximumof1100°C,inastreamofreducing gas,typicallylowconcentrationhydrogenorcarbonmonoxide balanced with an inert carrier. Reductionofthesampleisthenrecordedusingathermal conductivitydetector(TCD)astheconcentrationofthereducing gascomponentfallsasitisconsumedduringreductionofthe sample.AtMCAServices,theTCDiscalibratedwithrespectto reducinggasconcentrationwhichallowsforthecalculationof active gas consumption during the reduction process. AnalogoustoTPR,temperatureprogrammedoxidationisapplied tothestudyofoxidisablespeciesonamaterialsurface.The analyticalprocessisverysimilartothatofTPRwithoxygen replacing the reducing gas species in the carrier stream.
Temperature Programmed Reduction (TPR) & Temperaure Programmed Oxidation (TPO)
Static chemisorption analysisDynamic (pulse) chemisorption analysisWide choice of analysis temperaturesChoice of adsorbate: H2, CO & N2OWide choice and flexibility of pre-reduction conditionsActive species dispersion (%)Active species surface area and total sample surface areaActive species crystallite sizeComplimentary characterisations by Temperature Programmed AnalysisComplimentary Heat of Adsorption analysis
Analytical Options and Highlights
At MCA Services we use a state-of-the-art Micromeritics AutoChem II instrument which ensures analyses of great flexibility and precision. Dynamic, or pulse chemisorption is undertaken at atmospheric pressure using a flowing gas stream of an inert carrier. Successive injections of a calibrated volume of the chosen adsorbate gas are then made to the carrier gas and a Thermal Conductivity Detector is used to measure the volume of the injection not chemically adsorbed to the sample material. Analysis is complete when no further adsorbate is chemically adsorbed to the sample material. The total volume of chemically adsorbed probe molecule can the be ascertained and calculations of active metal dispersion, active metal surface area and crystallite size can be made.
Characterisation of availability of active speciesProduct formulation and process controlQC control of fabrication processesPerformance determination: efficiency and capacityAssessment of chemical activityDetermination of performance loss of time and useSuccess of re-generation processesStandard analyses using CO and H2 probe moleculesSpecialised probe molecules: N2O for Cu analysis
Key Applications
Chemisorption,alsoknownaschemicaladsorption,concernstheformationofchemicalbondsbetweenan adsorbatespeciesandtheactivesurfaceofasamplematerial.Chemisorptionisparticularlysuitedtothe characterisationandoptimisationofcatalystsbutitcanalsobeappliedtovirtuallyanymetalcontaining speciesonaninertsupportmaterial,irrespectiveofitsapplication.Chemisorptionanalysisprovides essentialinformationonactivemetalsurfacearea,dispersionandcrystallitesize.Essentially,thiscanbe usedtodeterminetheavailabilityoftheactivespecieswhichdirectlydeterminesefficiency,efficacyand capacity.Suchinvestigationsareapplicablethroughoutaproductslife-cycle,fromthefabricationprocess to investigating degradation during use and ultimately the success of a regeneration process.ChemisorptionisalsoextendedtoTemperatureProgrammedAnalysis:TemperatureProgrammed Reduction, Oxidation and Desorption and also the measurement of iso-steric Heat of Adsorption.
CHEMISORPTION
Multi-point BET surface area measurementSingle-point BET surface area option availableNitrogen and Krypton adsorption options cover virtually any surface areaReliable low pressure data applicable to highly micro-porous samplesComprehensive sample preparation and degassing optionsHighly adaptable methods to suit and match historical dataNumerical and graphical reporting format
Analytical Options and Highlights
AtMCAServicessampleanalysisisundertakenusingourMicromeriticsTriStar3030plusand3020 instruments,whichutilisethevolumetricmethodofgasadsorption.Beforeanalysisitisessentialthat samplesarefullydriedanddegassedasextraneoussubstanceswillprovideanartificiallylowsurface areavalue.Wehaveacomprehensiverangeofdegassingoptions,capableoftemperaturesintherange ambientto400°Cunderdynamicvacuumorflowinginertgas.Wecan,therefore,preparevirtuallyany samplematerialon-siteimmediatelypriortoanalysis,whichensuresthatthemostaccurateandreliable measurements are obtained.
Surface area directs the interaction of a solid with other mediaSurface Area is a critical factor for:Material selectionProcessing and fabrication method developmentRoutine QC of raw materials and finished productsPerformance assessment of products and materialsIdentification of performance issuesProduct capacity and life-cycleProduct regenerationAssessment of chemical activity
Key Applications
Thesurfaceareaofamaterialwilloftenprofoundlyaffectitsbehaviourandperformance,whateverits application.Therefore,understandingsurfaceareaiscommonlyacriticalparameterwhenconsidering materialsprocurement,processingandfabrication,assessmentofperformanceandinvestigationof atypicalperformanceandproductfailure.Specificsurfaceareacanbeusedtodirectlydeterminemany factors,suchasreactivity,adsorptioncapacity,dissolutionrate,electrochemicalandcatalytic performanceandsinteringability.SpecificsurfaceareaiscommonlymeasuredusingtheBET(Brunauer-Emmett-Teller)methodappliedtoagasadsorptionisotherm.Forthemajorityofmaterialsnitrogengas adsorptionisapplied,whichcanbecombinedwiththemoreextensivefullisothermanalysistodetermine poresizeandvolumecharacteristics.However,forverylowsurfaceareamaterialskryptongasadsorption becomesmorereliableandcanbeusedtodeterminesurfaceareaveryclosetothegeometricareaofa non-porous sample material.ThecombinationofnitrogenandkryptonadsorptionmethodsprovidesMCAServiceswiththecapabilityof accurately measuring materials with specific surface areas below 0.01 m2/g to over 2000 m2/g.
AtMCAServicesweapplythelateststate-of-the-art instrumentationtoourmaterialsanalysisoptions.Combined withdecadesofexperienceinouranalyticaltechniques acrossawiderangeofapplicationsandsectorsyouare assuredhighqualityanalysesandexpertdatainterpretation withthemostpertinentinformationtoobtainmaximum knowledge of your samples and their applications.
Temperatureprogrammeddesorptionisused tostudythetemperaturedependenceand strengthofinteractionbetweenasample surfaceandaprobemolecule.Typicalprobe moleculesincludeH2,CO2andNH3,although others,includingvapours,canalsobeapplied inordertoinvestigatespecificsystems.Initial adsorption,eitherphysicalorchemical,is usuallyconductedatambienttemperature, althoughsub-ambientconditionscanalsobe applied.Thedesorptionprocessisthen measuredwithsteadyincreasingsample temperature under inert gas flow. Recordingthetemperatureatwhich desorptionoccursandaccuratelymeasuring thevolumeofgasdesorbingallowsforthe determinationofthenumberandstrengthof activeadsorptionsitesonasamplesurface. Temperatureprogrammeddesorptioncanalso beextendedtoinvestigatesamplematerials whentheadsorption/desorptionprocesses aresignificanttoperformance,forexample effectivenessandregenerationofadsorbents, filtermaterialsandcatalystsandthesorption capacity of storage materials.
Temperature Programmed Desporption (TPD)
Our temperature programmed analyses are part of our suite of chemisorption options, used to investigate reduction, oxidation, desorption and decomposition as a function of temperature. Traditionally these have been applied to the catalysis sector where the understanding of surface reactions are fundamental to the development and regeneration of high efficiency systems. The use of these techniques is now commonly extended to other sectors and applications, particularly hydrogen storage and carbon capture. Temperature programmed analyses at MCA Services are undertaken using our state-of-the-art Micromeritics AutoChem II instrument, capable of analyses from sub-ambient (-70 °C) to 1100 °C. Furthermore, this instrument provides tremendous scope for accurate selection and control over analytical parameters such as gas flow rate, temperature ramp rate and temperature holding ranges. The instrument detector is always calibrated to match specific analytical parameters, ensuring the accurate calculation of active gas consumption.
Temperature Programmed Reduction (TPR) & Temperaure Programmed Oxidation (TPO)
Static chemisorption analysisDynamic (pulse) chemisorption analysisWide choice of analysis temperaturesChoice of adsorbate: H2, CO & N2OWide choice and flexibility of pre-reduction conditionsActive species dispersion (%)Active species surface area and total sample surface areaActive species crystallite sizeComplimentary characterisations by Temperature Programmed AnalysisComplimentary Heat of Adsorption analysis
Analytical Options and Highlights
At MCA Services we use a state-of-the-art Micromeritics AutoChem II instrument which ensures analyses of great flexibility and precision. Dynamic, or pulse chemisorption is undertaken at atmospheric pressure using a flowing gas stream of an inert carrier. Successive injections of a calibrated volume of the chosen adsorbate gas are then made to the carrier gas and a Thermal Conductivity Detector is used to measure the volume of the injection not chemically adsorbed to the sample material. Analysis is complete when no further adsorbate is chemically adsorbed to the sample material. The total volume of chemically adsorbed probe molecule can the be ascertained and calculations of active metal dispersion, active metal surface area and crystallite size can be made.
Characterisation of availability of active speciesProduct formulation and process controlQC control of fabrication processesPerformance determination: efficiency and capacityAssessment of chemical activityDetermination of performance loss of time and useSuccess of re-generation processesStandard analyses using CO and H2 probe moleculesSpecialised probe molecules: N2O for Cu analysis
Key Applications
Chemisorption,alsoknownaschemicaladsorption,concernsthe formationofchemicalbondsbetweenanadsorbatespeciesandthe activesurfaceofasamplematerial.Chemisorptionisparticularlysuited tothecharacterisationandoptimisationofcatalystsbutitcanalsobe appliedtovirtuallyanymetalcontainingspeciesonaninertsupport material,irrespectiveofitsapplication.Chemisorptionanalysis providesessentialinformationonactivemetalsurfacearea,dispersion andcrystallitesize.Essentially,thiscanbeusedtodeterminethe availabilityoftheactivespecieswhichdirectlydeterminesefficiency, efficacyandcapacity.Suchinvestigationsareapplicablethroughouta productslife-cycle,fromthefabricationprocesstoinvestigating degradationduringuseandultimatelythesuccessofaregeneration process.ChemisorptionisalsoextendedtoTemperatureProgrammedAnalysis: TemperatureProgrammedReduction,OxidationandDesorptionandalso the measurement of iso-steric Heat of Adsorption.
Forheliumpycnometryanalysis,MCAServiceshasarangeofsample cellswhichallowfortheaccuratedeterminationofabsolutedensity usingsamplesquantitiesfrom1cm3to10cm3.Itis,therefore,possible toanalyseawiderangeofsampletypes,fromfinepowderstolarger solidpieces.Ifthetheoreticalabsolutedensityofasamplematerialis knownitisalsopossibletocalculatethevolumeofclosedporeswithin thesamplefromtheheliumpycnometryvalue.Suchcalculationis especiallyusefulwhenconsideringfoamandconstructionmaterialsas it represents the void volume within the sample material.
Investigation of relationship between solid sample and fluid mediaPassage and retention capabilities of fluids and gases in solid materials:
Key Applications
Geological and geo-technical testingPetrology and HydrologyBattery electrodes: electrolyte flow and active site accessibilityBattery separators: electrolyte flow propertiesCatalyst testing: accessibility to active sitesPharmaceuticals: dissolution and disintegration propertiesFilter media: flow and retention propertiesMembranes and papers: flow throughout propertiesCeramics: flow throughput and capacity properties
Sample permeability and tortuosity measurement is offered as an extension to our standard mercury porosimetry analysis options, obtaining porosity and permeability information in a single analysis which provides a wealth of information in a short timeframe. Permeability is a measure of fluid or gas flow through a porous solid sample. It is, therefore, of considerable interest in applications where a solid material interacts with a liquid or gas. Permeability measurement from mercury intrusion analysis was originally developed with regard to geological samples, but it has since found significant application to a wide variety of sample types and sectors. Pore tortuosity, obtained from characteristics of pore size, pore volume, pore area and permeability is a measure of the tortuous pathway of pores through a sample: essentially a representation of how direct the pore pathway is as it passes through a sample. This can be particularly useful when comparing samples.
Pore volume (numerical and graphical reports)Pore Size Distribution (numerical and graphical reports)Pore Area (numerical and graphical reports)Average pore size by numerous calculationsAdditional calculation of bulk and skeletal densityAdditional calculation of absolute porosity (% volume)Characterisation of inter-particulate and intra-particulate porosityPermeability and Tortuosity measurementMercury intrusion and intrusion / extrusion optionsPore geometry assessment and cavity-to-throat size ratioAssessment of particle size via Mayer-Stowe methodExtensive and flexible reporting options
Analytical Options and Highlights
Mercuryporosimetryisanexceptionallypowerfulanalyticaltechnique forstudyingmaterialswithporosityinthemesoporeandmacropore ranges.AtMCAServicesweusethelatest,state-of-the-art MicromeriticsAutoPoreVinstrumenttoofferacomprehensivelistof flexibleanalyticalandreportingoptions.Combinedwithourdecadesof experience,weareabletorecommendandtailoranalysestoyour materialsandtheirperformanceinspecificapplications.Wearealso happytoassistwithdatainterpretationsothatyoureceivethemost pertinentdataandgainthemaximuminsightintoyourmaterialsand theirefficiency.Moreinformationaboutmercuryporosimetry,itsuse and background theory, is available on our YouTube channel.
Analysis of wide range of pore sizes 3.5nm to 650 µmApplicable to almost any solid sample formDissolution rate of pharmaceutical tablets and granulesPharmaceutical powder blends and resulting solid dose formsAssessment of powder inter-particulate size and volumeCeramic raw material and finished product characterisationEfficiency and efficacy of filter mediaChemical activity of catalysts and electrocatalystsFabrication of battery electrode, separator and solid electrolytesCapacity and efficiency of battery electrodes and materialsProduction and performance of construction materialsProduction and performance of coatings and abrasivesCharacterisation of geological samples and fluid interactionsProduct life-cycle and capacity assessmentInvestigations of atypical performance and failures
Key Applications
Mercury porosimetry provides a wealth of information for understanding the porous characteristics of any material with porosity in the size range 3.5 nm to 650 µm. The technique is applicable to virtually any solid form, from powders, through granules to single solid pieces, films, membranes, fabrics and coatings. The pore volume, pore area and pore size present in solid materials and between the particles of powder and granules often profoundly affect the fabrication and performance of materials. Porosity influences the efficiency, efficacy and functionality of materials across sectors such as pharmaceuticals, catalysis, energy production and storage, sorption technology and geology & environmental science and construction. It is usually necessary to consider the extent, nature and effects of porosity at all stages of product life-cycle, from the characterisation of raw materials, through formulation and fabrication processes to final use and application. Knowledge of the full porous character of materials is, therefore, critical to the understanding of materials and their application.
AtMCAServicessampleanalysisisundertakenusingourMicromeritics TriStar3030plusand3020instrument,combinedwithcomprehensive sampledegassingoptionscapableoftemperaturesintherange ambientto400°Cunderdynamicvacuumorflowinginertgas.Wecan, therefore,preparevirtuallyanysamplematerialon-siteimmediately priortoanalysis,whichensuresthemostaccurateandreliable measurements are obtained.
Pore volume, area and size distributions – numerically and graphicallyFull gas adsorption and desorption isotherm measurementDetermination of pore geometryBET Specific Surface Area includedAssessment of microporosity via t-plot analysis and DFT / NL-DFTExtensive and flexible analytical and reporting optionsExtensive and flexible sample degassing optionsAvailability of alternative adsorbents: argon and carbon dioxideComprehensive range of data reduction optionsBET Surface AreaBJH Mesopore volume, area and size – adsorption isothermBJH Mesopore volume, area and size – desorption isothermt-plot and α-S plot methodsDFT and NL-DFTLangmuir Surface AreaAssessment of pore geometry from isotherm hysteresisCombination with mercury porosimetry to extend pore size range to 650 µm
Adsorption capacity and efficacy of adsorbates and filter mediaActivity of catalysts and catalytic processesAssessment of new, spent and regenerated catalysts and filter mediaElectrochemical activity of battery components and constituentsFabrication process development and controlAvailability of biologically available sites in pharmaceuticalsInorganic, alumina and silica precursor and raw material assessmentBehaviour of powder materials for inclusion to pastes and emulsionsRaw material selection and QC processDissolution and dispersion assessment and controlRapid assessment of microporous materials
Poresizescanbedividedintothreeranges:Micropores(<2nm),Mesopores(2–50nm)andMacropores(> 50nm),thesizesrefertothediameterofacylindrical poreorthewidthofaslit-shapedporeaccordingto IUPACdefinitions.Micro-poresaresometimesfurther dividedtoincludesuper-micropores,orultra-microporeswhicharesmallerthan1nm.Poregeometry, whichincludestypesandshapesofporesshouldalso be considered.Thereisnosingletechniquethatcanbeusedto determineporouscharacteristicsthroughouttheranges ofporesizes.Therefore,itisusuallynecessarytoselect themostappropriatetechniqueorcombinationof techniquesforagivensampleandapplication.AtMCA Serviceswehavedecadesofexperienceinthisandare always happy to provide our thoughts on this selection.
Porosimetrycoversarangeofanalyticaltechniquesusedfor understandingandcharacterisingtheporousnatureofmaterials. Porosityoftenhasprofoundaffectsonthebehaviourofmaterialsand influencesmanyaspectsoftheirselection,fabrication,application, performance and life-cycle. Porosityisabroadtermwhichencompassesphysicalcharacteristics suchasporevolume,poresurfacearea,poresizedistribution,specific surfacearea,absoluteporosityandporegeometry.Italsohasdirect relationshipswiththevariousmeasuresofsampledensity,gasand fluidpermeabilityandchemicalactivity.Alloftheseaspectsofporosity canbecharacterisedatMCAServicesusingarangeofstate-of-the-art analyticalinstruments.Ourexpertiseintheapplicationofanalysesand interpretationmeansthatthemostpertinentdataispresentedand related directly to specific materials and applications. Porosityiscommonlyconsideredasbeingpresentwithinasolid materialbutitisalsopresentinthevoidspacesofapowdermaterial. Suchinter-particulateporosityisdeterminedbytheparticlesizeand shapeofthepowdergrains,essentiallyreflectingthepacking propertiesofpowderparticles.Understandinginter-particulateporosity becomesverysignificantwhenapowderisusedinthefabricationofa solidarticle.Combinedwiththeprocessconditions,suchas compression,bindercompositionandfiringtemperatureitdetermines the porosity within the finished article.
Multi-point BET surface area measurementSingle-point BET surface area option availableNitrogen and Krypton adsorption options cover virtually any surface areaReliable low pressure data applicable to highly micro-porous samplesComprehensive sample preparation and degassing optionsHighly adaptable methods to suit and match historical dataNumerical and graphical reporting format
Surface area directs the interaction of a solid with other mediaSurface Area is a critical factor for:Material selectionProcessing and fabrication method developmentRoutine QC of raw materials and finished productsPerformance assessment of products and materialsIdentification of performance issuesProduct capacity and life-cycleProduct regenerationAssessment of chemical activity
Key Applications
Thesurfaceareaofamaterialwilloftenprofoundlyaffectitsbehaviour andperformance,whateveritsapplication.Therefore,understandingsurfaceareaiscommonlyacriticalparameterwhenconsidering materialsprocurement,processingandfabrication,assessmentof performanceandinvestigationofatypicalperformanceandproduct failure.Specificsurfaceareacanbeusedtodirectlydeterminemany factors,suchasreactivity,adsorptioncapacity,dissolutionrate, electrochemicalandcatalyticperformanceandsinteringability. SpecificsurfaceareaiscommonlymeasuredusingtheBET(Brunauer-Emmett-Teller)methodappliedtoagasadsorptionisotherm.Forthe majorityofmaterialsnitrogengasadsorptionisapplied,whichcanbe combinedwiththemoreextensivefullisothermanalysistodetermine poresizeandvolumecharacteristics.However,forverylowsurface areamaterialskryptongasadsorptionbecomesmorereliableandcan beusedtodeterminesurfaceareaveryclosetothegeometricareaofa non-porous sample material.Thecombinationofnitrogenandkryptonadsorptionmethodsprovides MCAServiceswiththecapabilityofaccuratelymeasuringmaterials with specific surface areas below 0.01 m2/g to over 2000 m2/g.