Thermal testing, thermo mechanical and dynamic mechanical analysis & chemical testing, unit-v; testing of materials

Unit-V: THERMAL TESTING, THERMO-MECHANICAL AND DYNAMIC MECHANICAL ANALYSIS & CHEMICAL TESTING [OTHER TESTING].
Subject Name: OML751 Testing of Materials
Topics: Thermal Testing: Differential scanning calorimetry, Differential thermal analysis. Thermo-mechanical and Dynamic mechanical analysis: Principles, Advantages, Applications. Chemical Testing: X-Ray Fluorescence, Elemental Analysis by Inductively Coupled Plasma-Optical Emission Spectroscopy and Plasma-Mass Spectrometry.
B.E. Mechanical Engineering
Final Year, VII Semester, Open Elective Subject
[As per Anna University R-2017]

1. OML751 -TESTING OF MATERIALS
VII SEMESTER
[R 2017 -Open Elective Subject]
©S.Thirumalvalavan, Assistant Professor,
Department of Mechanical Engineering,
E-Mail : [email protected]
UNIT V -OTHER TESTING
THERMAL TESTING, THERMO-MECHANICAL AND
DYNAMIC MECHANICAL ANALYSIS & CHEMICAL TESTING
1

2. OML751 –TESTING OF MATERIALS -SYLLABUS
UNITV OTHERTESTING 9
ThermalTesting:Differentialscanningcalorimetry,Differentialthermalanalysis.Thermo-
mechanicalandDynamicmechanicalanalysis:Principles,Advantages,Applications.Chemical
Testing:X-RayFluorescence,ElementalAnalysisbyInductivelyCoupledPlasma-Optical
EmissionSpectroscopyandPlasma-MassSpectrometry.
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3. UNIT-V : OTHER TESTING
ThermalTesting:
Differentialscanningcalorimetry
Differentialthermalanalysis.
Thermo-mechanicalandDynamicmechanicalanalysis:
Principles,Advantages,Applications
ChemicalTesting:
X-RayFluorescence,
ElementalAnalysisbyInductivelyCoupledPlasma-OpticalEmissionSpectroscopy&
Plasma-MassSpectrometry.
3https://www.slideshare.net/ThirumalValavan2/

4. Materialtesting,measurementofthecharacteristicsandbehaviorofsuchsubstancesas
metals,ceramicsorplasticsetc.,undervariousconditions.
Investigatorsmayconstructmathematicalmodelsthatutilizeknownmaterialcharacteristics
andbehaviourtopredictcapabilitiesofthestructure.
Overview
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5. Materialstestingbreaksdownintomajorcategories
MechanicalTesting&NonDestructiveTesting
Testingforphysical&chemicalproperties
Testingforthermalproperties
Testingforelectricalproperties
Testingforresistancetocorrosion,Radiationandbiologicaldeterioration
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6. Thermalanalysisisaformofanalyticaltechniquemostcommonlyusedinthebranchof
materialssciencewherechangesinthepropertiesofmaterialsareexaminedwithrespectto
temperature.
Itisagroupoftechniquesinwhichchangesofphysicalorchemicalpropertiesofthesampleare
monitoredagainsttimeortemperature,whilethetemperatureofthesampleisprogrammed.
Thetemperatureprogrammayinvolveheatingorcoolingatafixedrate,holdingthe
temperatureconstant(isothermal),oranysequenceofthese.
Thesampleissubjectedtoapredefinedheatingorcoolingprogram.
Thesampleisusuallyinthesolidstateandthechangesthatoccuronheatingincludemelting,
phasetransition,sublimationanddecomposition.
THERMAL ANALYSIS
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7. ThermalAnalysis(TA)isagroupoftechniquesinwhichchangesofphysicalorchemicalpropertiesofthe
samplearemonitoredagainsttimeortemperature,whilethetemperatureofthesampleisprogrammed.
Thetemperatureprogrammayinvolveheatingorcoolingatafixedrate,holdingthe
temperatureconstant(isothermal),oranysequenceofthese.
Thesampleissubjectedtoapredefinedheatingorcoolingprogram.
Thesampleisusuallyinthesolidstateandthechangesthatoccuronheatingincludemelting,phase
transition,sublimation,anddecomposition.
Application of thermal analysis in characterization ofsolids
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8. Thermalconductivity
Specificheat
Thermalexpansion
Thermalstress
Thermo-Elasticeffect
Thermalshock
Meltingpointorheatresistance
Emissivityofmaterials
Latentheatoffusionofmaterials
Latentheatofvaporizationofmaterials
Thermal Properties
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9. Thermaltestinginvolvestestingaproductattheextremesofitsintendedusethermal
environmentforheatingrate,temperatureandairfloworgaseousatmosphereorvacuum
withmeasuringcasetemperaturesonindividualcomponentstodeterminetheeffecton
productperformanceandlong-termreliability.
Itmeasuresbasedondynamicrelationshipbetweentemperature,mass,volumeandheat
ofreaction.
THERMAL TESTING
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10. Differentialthermalanalysis
Dilatometer
Differentialscanningcalorimetry
Dynamicmechanicalanalysis
Thermogravimetricanalysis
Thermomechanicalanalysis
Thermoopticalanalysis
Major methods of Thermal testing
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Othercommonmethodofthermalmethods
Dielectricthermalanalysis
Evlovedgasanalysis
Laserflashanalysis
Derivatography

11. Parameters of Thermal testing
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SI.No METHOD PARAMETER TESTING
1ThermogravimetricAnalysis Mass changes
2Differential Thermal Analysis Temperature Difference
3Differential Scanning Calorimetry Heat Difference
4Evolved Gas Analysis Gas Decomposition
5Thermo MechanicalAnalysis Deformationand Dimension
6Dilatometer Volume
7Dielectric thermal analysis Electrical properties
8Thermo optical analysis Optical properties

12. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 12
DifferentialThermalAnalysis(DTA):Thetemperaturedifferencebetweenasampleandaninertreference
material,ΔT=TS-TR,ismeasuredasbotharesubjectedtoidenticalheattreatments.
DifferentialScanningCalorimetry(DSC):Thesampleandreferencearemaintainedatthesametemperature,
evenduringathermalevent(inthesample).Theenergyrequiredtomaintainzerotemperaturedifferential
betweenthesampleandthereference,dΔq/dt,ismeasured.
ThermogravimetricAnalysis(TGA):Thechangeinmassofasampleonheatingismeasured
Dynamic Mechanical Analysis: Viscoelastic Properties
Thermo mechanical Analysis: Thermal Expansion Coefficient
Dielectric Thermal Analysis
Evolved Gas Analysis
Thermo-Optical Analysis
Dilatometry
Types of Thermal Analysis Techniques

13. TheTGAisatypeofthermoanalyticaltestingperformedonmaterialstodeterminechanges
inweightinrelationtochangesintemperature.
TheTGAreliesonahighdegreeofprecisioninthreemeasurements:Weight,Temperature
andTemperaturechange.
TheTGAiscommonlyemployedinresearchandtestingtodeterminecharacteristicsof
materials,todeterminedegradationtemperatures,absorbedmoisturecontentofmaterials,
thelevelofinorganicandorganiccomponentsinmaterials,decompositionpointsof
explosivesandsolventresidues.
THERMOGRAVIMETRIC ANALYSIS (TGA)
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14. 14
1.DIFFERENTIAL SCANNING CALORIMETRY (DSC)
2.DIFFERENTIAL THERMAL ANALYSIS (DTA)
https://www.slideshare.net/ThirumalValavan2/

15. DSCmeasurestheenergyabsorbedorreleasedfromasampleasafunctionoftimeora
temperatureprofile.
DSCisusefultomakethemeasurementsformeltingpoints,heatsofreaction,glass
transition,andheatcapacity.
DIFFERENTIAL SCANNING CALORIMETRY (DSC)
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16. DSCisbasedontheprinciple,sampleandreferencearemaintainedatthe
sametemperature,evenduringathermalevent(inthesample).Theenergy
requiredmaintainingzerotemperaturedifferentbetweenthesampleandthe
referenceismeasured.
Bycalibratingthestandardmaterials(referencematerial),theunknown
samplequantitativemeasurementisachievable.
DSC –PRINCIPLE
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17. Power compensation DSC Heat fluxDSC
PRINCIPLE:DSCdiffersfundamentallyfromDTAinthatthesampleandreferencearebothmaintainedatthe
temperaturepredeterminedbytheprogram(i.e.ΔTofreference/sampleismaintained@0)
Duringathermaleventinthesample,thesystemwilltransferheattoorfromthesamplepantomaintainthesame
temperatureinreferenceandsamplepans.
Currentrequiredtomaintainisothermalconditionsisrecorded
Endothermicprocesseswilllowerthesampletemperaturerelativetothatofreference,sothesamplemustbe
heatedmoreinordertomaintainequalTinbothpans
TwobasictypesofDSCinstruments:powercompensationandheat-flux
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18. TherearefivedifferenttypesofDSCinstrument
HeatfluxDSC
PowercompensatedDSC
ModulatedDSC
HyperDSC
PressureDSC
ThemostcommonmethodsarePowercompensatedDSC&HeatfluxDSC
DIFFERENTIAL SCANNING CALORIMETRY (DSC) -TYPES
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19. Temperaturesofthesampleandreferencearecontrolledindependentlyusingseparate,identicalfurnaces.
Thetemperaturesofthesampleandreferencearemadeidenticalbyvaryingthepowerinputtothetwofurnaces;the
energyrequiredtodothisisameasureoftheenthalpyorheatcapacitychangesinthesamplerelativetothereference.
Sample holder:Al or Platinum pans
Sensors
Pt resistance thermocouples
separate sensors and heaters for the sample and reference
Furnace
Separate blocksfor sampleand reference
cells
Temperature controller
differential thermal power is supplied to the heaters to maintain
the temperature of the sample and reference at the program value
Power CompensationDSC
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20. •Thepowerneededtomaintainthesampletemperatureequaltothereference
temperatureismeasured.
•InpowercompensationDSCtwoindependentheatingunitsareemployed.
•Theseheatingunitsarequitesmall,allowingforrapidratesofheating,coolingand
equilibration.Theheatingunitsareembeddedinalargetemperature-controlledheatsink.
•Thesampleandreferenceholdershaveplatinumresistancethermometerstocontinuously
monitorthetemperatureofthematerials.
•Theinstrumentrecordsthepowerdifferenceneededtomaintainthesampleand
referenceatthesametemperatureasafunctionoftheprogrammedtemperatures.
Working
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21. •PowercompensatedDSChaslowersensitivitythanheatfluxDSC,butitsresponsetimeis
morerapid.ItisalsocapableofhigherresolutionthenheatfluxDSC.
•ThismakespowercompensatedDSCwellsuitedforkineticsstudiesinwhichfast
equilibrationstonewtemperaturesettingareneeded.
Working
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22. Sampleandreferenceareconnectedbyalowresistanceheatflowpath(ametaldisc).Theassemblyisenclosedina
singlefurnace.
Enthalpyorheatcapacitychangesinthesamplecauseadifferenceinitstemperaturerelativetothereference;the
resultingheatflowissmallcomparedwiththatindifferentialthermalanalysis(DTA)becausethesampleandreference
areingoodthermalcontact.
Thetemperaturedifferenceisrecordedandrelatedtoenthalpychangeinthesampleusingcalibrationexperiments
HEAT FLUXDSC
One blocks for both sample and reference cells
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23. HEAT FLUXDSC
Sampleholder
Sampleandreferenceareconnectedbyalow-resistanceheatflowpath
AlorPtpansplacedonconstantandisc
Sensors:Chromel®-alumelthermocouples
Furnace
Oneblockforbothsampleandreferencecells
Heatingblockdissipatesheattothesample
andreferenceviatheconstantandisc
One blocks for both sample and reference cells
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25. •ThemainassemblyoftheDSCcellisenclosedinacylindrical,silverheatingblack,which
dissipatesheattothespecimensviaaconstantandiscwhichisattachedtothesilver
block.
•Thediskhastworaisedplatformsonwhichthesampleandreferencepansareplaced.
•Achromeldiskandconnectingwireareattachedtotheundersideofeachplatform,and
theresultingchromel-constantanthermocouplesareusedtodeterminethedifferential
temperaturesofinterest.
•Alumelwiresattachedtothechromediscsprovidethechromel-alumeljunctionsfor
independentlymeasuringthesampleandreferencetemperature.
WORKING
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26. •Glasstransitions
•Meltingandboilingpoints
•Crystallizationtimeandtemperature
•Percentcrystallinity
•Heatsoffusionandreactions
•Specificheatcapacity
•Oxidative/thermalstability
•Reactionkinetics
•Purity
DSC –Measures
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27. Temperaturecontroller
Thetemperaturedifferencebetweenthesampleandreferenceisconvertedtodifferentialthermalpower,
dΔq/dt,whichissuppliedtotheheaterstomaintainthetemperatureofthesampleandreferenceattheprogram
value
Temperature,K
dH/dt,
mJ/s
Thermogram
exo
Glass transition
melting
crystallization
endo
Output ofDSC
DSC Curve
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28. Factors affecting DSC Curve
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29. Calibration
Contamination
Samplepreparation–howsampleisloadedintoapan
Residualsolventsandmoisture
Thermallag
Heating/coolingrates
Samplemass
SOURCES OF ERRORS
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30. •Instrumentscanbeusedatveryhightemperatures
•Instrumentsarehighlysensitive
•Flexibilityinsamplevolume/form
•Highresolutionobtained
•Highsensitivity
•Stabilityofthematerial.
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Advantages of DSC

31. •DSCgenerallyunsuitablefortwo-phasemixtures
•Difficultiesintestcellpreparationinavoidingevaporationofvolatile
solvents.
•DSCisgenerallyonlyusedforthermalscreeningofisolatedintermediates
andproducts
•Doesnotdetectgasgeneration
•Uncertaintyofheatsoffusionandtransitiontemperatures.
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Limitations of DSC

32. Toobservefusionandcrystallizationeventsaswellglasstransitiontemperature
Tostudyoxidation,aswellasotherchemicalreactions
Glasstransitionmayoccurasthetemperatureofanamorphoussolidisincreased.Thesetransition
appearasastepinthebaselineoftherecordedDSCsignal.Thisisduetothesampleundergoinga
changeinheatcapacity.
Asthetemperatureincreases,anamorphoussolidwillbecomelessviscous.Atsomepointthe
moleculesmayobtainenoughfreedomofmotiontospontaneouslyarrangethemselvesintoa
crystallineform.Thisisknownasthecrystallizationtemperature.Thistransitionfromamorphousto
crystallineisanexothermicprocess,andresultsinapeakintheDSCsignal.
Asthetemperatureincreasesthesampleeventfullyreachesitsmeltingpoint.Themeltingprocess
resultsinanendothermicpeakintheDSCcurve.
TheabilitytodeterminetransitiontemperatureandenthalpiesmakesDSCaninvaluabletollin
producingphasediagramforvariouschemicalsystems.
Application of DSC
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33. 2. DIFFERENTIAL THERMAL ANALYSIS (DTA)
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34. Differentialthermalanalysis(DTA)isathermo-analytical
techniquewhichisusedforthermalanalysiswherethermal
changescanbestudied.
Itisusedtodeterminetheoxidationprocess,decomposition,and
lossofwaterorsolvent
DIFFERENTIAL THERMAL ANALYSIS (DTA)
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35. PRINCIPLE:Atechniqueinwhichthetemperaturedifferencebetweena
substanceandreferencematerialismeasuredasafunctionoftemperature,
whilethesubstanceandreferencearesubjectedtoacontrolledtemperature
programme.
TherecordisthedifferentialthermalorDTAcurve;thetemperature
difference(ΔT)shouldbeplottedontheordinate(withendothermic
reactionsdownwardsandexothermicreactionsupwards)andtemperature
ortimeontheabscissaincreasingfromlefttoright.
Endothermicreaction(absorptionofenergy)includesvaporization,
sublimation,andabsorption&givesdownwardpeak.
Exothermicreaction(liberationofenergy)includesoxidation,
polymerization,andcatalyticreaction&givesupwardpeak.
DIFFERENTIAL THERMAL ANALYSIS (DTA)
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37. Furnace
Sampleholder
DCamplifier
Differentialtemperaturedetector(Thermogram)
Furnacetemperatureprogramme
Recorder
Controlequipment
DIFFERENTIAL THERMAL ANALYSIS (DTA) -COMPONENTS
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38. Specimens
Sample
Reference(Knownsubstance,thermallyinertoverthetemprangeofinterest)
Sample holder
Container for sample and reference
Sensors
Pt/Rhorchromel/alumelthermocouplesoneforthesampleandoneforthe
referencejoinedtodifferentialtemperaturecontroller
Furnace
Aluminablockcontainingsampleandreferencecells
Temperature controller/ Programmer
Controlsfortemperatureprogramandfurnaceatmosphere
Uniform heating rate: 10-20
o
/min
Recorder
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39. Thesampleunderinvestigationisloadedintoacontainer
ThiscontaineristhenplacedontothesamplepananditismarkedasS(meansample).
Samequantityofreferencesampleisplacedinanothercontainerwhichisthenplacedonto
thereferencepananditismarkedasR(meansreference).
Inordertoheatthesamplepanandthereferencepanatanidenticalrate,thedimensions
ofthesetwopansshouldbenearlyidentical;moreover,thesampleandthereference
shouldhaveequalweights,thermallymatchedandshouldbearrangedsymmetricallywith
thefurnace.
Themetalblockwhichsurroundsthepanactsasaheatsinkwhosetemperatureisincreased
slowlybyusinganinternalheater.
DIFFERENTIAL THERMAL ANALYSIS (DTA) -WORKING
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41. Thesinkthenheatsthesampleandreferencematerialsimultaneously.
Twopairsofthermocouplesareused,onepairisincontactwiththesampleandthesecond
pairisincontactwiththereference.
Thermocoupleisattachedwithanamplifierwhichamplifiestheresultofdifferential
thermocoupleandsentthisresulttotheread-outdevicewhichdisplaystheresultsinthe
formofDTAcurveorThermogramasfunctionofthesampletemperature,reference
temperatureortime.
Nosignalisgeneratedifnotemperaturedifferenceisobservedeventhoughtheactual
temperaturesofboththesampleandreferenceareincreasing.
DIFFERENTIAL THERMAL ANALYSIS (DTA) -WORKING
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42. Whenthereisaphysicalchangeinthesamplethenheatisabsorbedorreleased.
ForExample:whenametalcarbonateisdecomposedthencarbondioxideisreleased.This
isanendothermicreactionwheretheheatisabsorbedandthetemperatureofthesampleis
decreased.
Nowthesampleisatalowertemperaturethanthatofthereference.Thistemperature
differencebetweensampleandreferenceproducedanetsignal,whichisthenrecorded.
DIFFERENTIAL THERMAL ANALYSIS (DTA) -WORKING
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43. If S and R are heated at the same rate, by placing them in the same furnace, their temperatures will rise
TR rises steadily, as the reference material is chosen to have no physical or chemical transitions
TSalsorisessteadilyintheabsenceofanytransitions,butifforinstancethesamplemelts,itstemperaturewill
lagbehindTRasitabsorbstheheatenergynecessaryformelting
Ifanexothermic(heat-producing)eventhadoccurred,thecurvewouldshowapeakintheoppositedirection
TheareaAonthecurveisproportionaltotheheatofthereaction:ΔH=K.A=KʃΔT.dt
K=Proportionalityconstantandincludesthermalpropertiesofthesubstance
DTA Curve –Differential Thermal Analysis Plot
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44. DTA Curve
(a)The DTA curve or thermo gram is a plot
between differential temperature and time
(b) DTA curve may be endothermic (downward plot)
or exothermic (upward plot)
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45. Factors affecting DTA Curve
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46. Advantages:
Instruments can be used at very hightemperatures
Instruments are highly sensitive
Flexibility in cruciblevolume/form
Characteristic transition or reaction temperatures can be accuratelydetermined
Determination of transition temperatures are accurate in aDTA.
Disadvantages:
Estimates of enthalpies of transition are generally not accurate i.e. Uncertainty of
heatsof fusion, transition, or reaction ; estimations is 20-50%.
Advantages & Disadvantagesof DTA
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47. Applications of DTA
Rapid identification on the compositions of mixed clays
Polymers characteristics can be easily characterized
Degree of crystallinity can be measured
Qualitative and Quantitative Identification of Minerals: detection of any minerals in a
sample
Measures:
T
g (Glass transition temperature), T
m (Melting temperature), T
d (decomposition)
Heat of fusion, vaporization, crystallization,
Heat of reaction, decomposition, solution, adsorption
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48. Atechniqueinwhichadeformationofthesampleundernon-oscillatingstressis
monitoredagainsttimeortemperaturewhilethetemperatureofthesample,ina
specifiedatmosphere,isprogrammed.
Thermomechanicalanalysis(TMA)easilyandrapidlymeasuressampledisplacement
(growth,shrinkage,movement,etc..)asafunctionoftemperature,timeandapplied
force.
THERMO-MECHANICAL ANALYSIS (TMA)
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49. Thermomechanicalanalysis(TMA)isusedtomeasurethedimensionalchangesofa
materialasafunctionoftemperaturebyapplyingstress.Thestressmaybe
compression,tension,flexureortorsion.
THERMO-MECHANICAL ANALYSIS -PRINCIPLE
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50. Transducer–Linearvariabledisplacementtransducer(LVDT),Laseroptoelectronicetc.,
Probe(madeupofquartzglass)
Thermocouplefurnace
Forcegenerator
THERMO-MECHANICAL ANALYSIS -COMPONENTS
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51. PROBES ON DIFFERENT LOADING CONDITION
Loading Condition Load Application Purpose
(a) Expansion /
Compression Probe
It is used for the measurement of
the deformation by the thermal
expansion and the transition of the
sample under the compressed
force is applied.
(b) Penetration Probe
It is used for the measurement of
the softening temperature
(c) Tension Probe
It is used for the measurement of
the thermal expansion and the
thermal shrinkage of the sample
such as the film and the fiber.
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52. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 52

53. Thesampleisinsertedintothefurnaceandistouchedbytheprobewhichisconnected
withthelengthdetectorandtheforcegenerator.Theconstructionofthepushrodand
sampleholderdependsonthemodeofthemeasurements.
THERMO-MECHANICAL ANALYSIS –Construction & Working
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54. ThethermocoupleforTEMPERATUREMEASUREMENTISLOCATEDNEARTHESAMPLE.Therate
of5
o
C/minisusuallythemaximumrecommendedvalueforgoodtemperatureequilibration
acrossthespecimen.
Thesampletemperatureischangedinthefurnacebyapplyingtheforceontothesamplefrom
theforcegeneratorviaprobe.
Thesampledeformationsuchasthermalexpansionandsofteningwithchangingtemperature
ismeasuredastheprobedisplacementbythelengthdetector.LinearVariableDifferential
Transformer(LVDT)isusedforlengthdetectionsensor.
EverydisplacementofthepushrodistransformedintoananalogsignalbytheLVDT,converted
todigitalformandthenrecordedinthecomputersystem,andfinallypresentedbythe
softwareasadimensionalchangeversustimeortemperature.
THERMO-MECHANICAL ANALYSIS –Construction & Working
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55. •Measurementofdimensionalchange
•Coefficientoflinearthermalexpansion
•Determinationofmaterialanisotropy
•Softeningtemperaturesandglasstransition
•Linearthermalexpansion
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Applications

56. •Compactnessandlightness
•Lowoperationvoltage
•Measureslargedeformation
•Largeactuationforce
•Measuresrelaxationeffects
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Advantages

57. •Usedonlyforsolidsamples
•Creepoccurringconcurrentlywithnormaldimensionalchanges
•Usageofproperprobe
•Lowoperationalspeed
57
Limitations
https://www.slideshare.net/ThirumalValavan2/

58. Thermomechanicaldynamicanalysis,otherwiseknownasDynamicMechanical
Analysis(DMA),isatechniquewhereasmalldeformationisappliedtoasampleina
cyclicmanner.
Thisallowsthematerialsresponsetostress,temperature,frequencyandother
valuestobestudied.Thetermisalsousedtorefertotheanalyzerthatperforms
thetest.
Dynamicmechanicalanalysis(DMA)isanimportanttechniqueusedtomeasurethe
mechanicalandviscoelasticpropertiesofmaterialssuchasthermoplastics,
thermosets,elastomers,ceramicsandmetals.
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THERMO-MECHANICAL DYNAMIC ANALYSIS (DMA)

59. Asinusoidalstressisappliedandthestraininthematerialismeasured,allowing
onetodeterminethecomplexmodulus.
Thetemperatureofthesampleorthefrequencyofthestressareoftenvaried,
leadingtovariationsinthecomplexmodulus;thisapproachcanbeusedto
locatedthetemperatureofthematerial,aswellastoidentifytransitions
correspondingtoothermolecularmotions.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 59
THERMO-MECHANICAL DYNAMIC ANALYSIS -PRINCIPLE

60. Forcedresonanceanalyzers–Analyzersforcethesampletooscillateatacertain
frequencyandarereliableforperformingatemperaturesweep.
Freeresonanceanalyzers–Freeresonanceanalyzersmeasurethefree
oscillationsofdampingofthesamplebeingtestedbysuspendingandswinging
thesample.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 60
TYPES OF THERMO MECHANICAL DYNAMIC ANALYZER

61. Stress(force)control–Thestructureofthesampleislesslikelytobedestroyed
andlongerrelaxationtimes/longercreepstudiescanbedone.
Strain(displacement)control–Thebettershorttimeresponseformaterialsof
lowviscosityandexperimentsofstressrelaxationaredonewithrelativeease.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 61
MODE OF ANALYZER

62. TransducerSensor(LinearVariableDisplacementTransducerLVDT)–Itiswhich
measuresachangeinvoltage.
Driveshaftorprobe–Itisasupportandguidancesystemtoactasaguidefor
theforcefromthemotortothesample.
Drivemotor–Alinermotorforprobeloadingwhichprovidesloadforthe
appliedforce.
Steppermotor–Itcontrolsthespecimendimensionandmeasurement.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 62
COMPONENTS

63. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 63
Cross sectional of Thermo mechanical dynamic analyzer

64. ThesampleisclampedinthemeasurementheadoftheDMAinstrument.
Duringmeasurement,sinusoidalforceisappliedtothesampleviatheprobeor
drivingshaft.
Deformationcausedbythesinusoidalforceisdetectedandtherelation
betweenthedeformationandtheappliedforceismeasured.
Propertiessuchaselectricityandviscosityarecalculatedfromtheappliedstress
andstrainplottedasafunctionoftemperatureortime.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 64
THERMO-MECHANICAL DYNAMIC ANALYSIS –WORKING

65. DIFFERENT LOADING CONDITION
Modes Stress application Purpose
Shear mode
Used for evaluationof thin fibers or
films or bundle of single fiber
3-point bending mode
Bestfor medium to high modulus
materials.
Dual cantilever mode
Highly damped materials can be
measured.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 65

66. DIFFERENT LOADING CONDITION
Modes Stress application Purpose
Singlecantilever mode Suited best for thermoplastics
Tension or compression
mode
Used for low medium modulus
materials
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 66

67. •Themostsuitabletypeshouldbeselecteddependingonthesampleshape,
modulusandmeasurementpurpose.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 67
DIFFERENT LOADING MODES

68. •Displacementandforce
•Widerangeofforce1mNto40N
•Widerangeoffrequency0.001to1000Hz.
•Widestiffnessrange.
•Coefficientofthermalexpansion(CTE)
•GlassTransitionTemperature
•CompressionModulusofpolymericmaterials
•Viscoelasticpropertiessuchas:
Storagemodulus(purelyelasticcomponent)
Lossmodulus(purelyviscouscomponent)
Losstangent
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 68
DMA MEASURES

69. •Itisanessentialanalyticaltechniquetodeterminingtheviscoelasticpropertiesof
polymers.
•Verysoftandhardsamplesaremeasured.
•Allowsaccuratetemperaturemeasurement.
•Itcanprovidemajorandminortransitionsofmaterials
•Itisalsomoresensitive
•Itisabletoquicklyscanandcalculatethemodulusforarangeoftemperatures.
•Itistheonlytechniquethatcandeterminethebasicstructureofapolymer
system.
•Thisanalyticalmethodisabletoaccuratelypredicttheperformanceofmaterials
inuse.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 69
ADVANTAGES

70. •Itleadstocalculationinaccuracies.
•Thelargeinaccuraciesareintroducedifdimensionalmeasurementsofsamples
areslightlyinaccurate.
•Theoscillatingstressconvertsmechanicalenergytoheatandchangesthe
temperatureofthesample.
•Themaintaininganexacttemperatureisimportantintemperaturescans,this
alsointroducesinaccuracies.
•Thefinalsourceofmeasurementuncertaintycomesfromcomputererror.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 70
LIMITATIONS

71. •Measurementoftheglasstransitiontemperatureofpolymers
•Varyingthecompositionofmonomers
•Effectivelyevaluatethemiscibilityofpolymers
•Tocharacterizetheglasstransitiontemperatureofamaterial
•Mechanicalpropertiesintherelevantfrequencyrange
•Modulusinformation
•Nonlinearproperties
•Dampingbehaviour
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 71
APPLICATION

72. Chemicalanalysisisusedtoidentifythecontents,compositionandqualityof
thematerialsusedinproductdevelopment,manufacturingandtesting.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 72
CHEMICAL ANALYSIS

73. Achemicalpropertyisacharacteristicorbehaviorofasubstancethatmaybe
observedwhenitundergoesachemicalchangeorreaction.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 73
CHEMICAL PROPERTY

74. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 74

75. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 75

76. Chemicaltestingprovidesavarietyofquantitativeandqualitativeservicesfor
verification,identificationandcomponentanalysisofferrousandnon-ferrous
metals.
76
CHEMICAL TESTING
https://www.slideshare.net/ThirumalValavan2/

77. Chemicaltreeanalysis
Elementaltraceanalysis
Failureanalysis
Contaminationanalysis
Materialsanalysisandtesting
Materialverification
Materialidentification
Chemicalcompositionanalysis
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 77
PURPOSE OF CHEMICAL TESTING

78. (A)CHROMATOGRAPHYTECHNIQUE
Gaschromatography
Ionchromatography
Liquidchromatography
(B)MASSSPECTROSCOPYTECHNIQUE
GaschromatographyMassspectroscopy
Inductivelycoupledplasma
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 78
CHEMICAL COMPOSITION TECHNIQUE AND TESTS

79. (C)SPECTROSCOPYTECHNIQUE
Fourier-transforminfraredspectroscopy
X-ray–EDS&XRFanalysis
Inductivelycoupledplasma(ICP-AES)
Atomicabsorptiongraphitefurnace(GF-AAS)
Sparkatomicemissions(Spark-AES)
(D)WETCHEMISTRYTECHNIQUE
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 79
CHEMICAL COMPOSITION TECHNIQUE AND TESTS

80. 80
CHEMICAL COMPOSITION TECHNIQUE AND TESTS
Chemical
Composition
Tests
Chromatography
Technique
Mass Spectroscopy
Technique
Spectroscopy
Technique
Wet Chemistry
Technique
1.Gas Chromatography
2.Ion Chromatography
3.Liquid Chromatography
1.Gas Chromatography Mass
Spectroscopy
2.Inductively Coupled Plasma
1.FTIR (Solution & Pellet)
2.X-ray –EDS & XRF analysis
3.Inductively Coupled Plasma
4.Atomic Absorption Graphic
Furnace
5.Spark Atomic Emissions
Types of chemical composition test@ S. Thirumalvalavan, AP/Mech, 5104 -AEC.

81. XRF(X-rayfluorescence)isanon-destructiveanalyticaltechniqueusedto
determinetheelementalcompositionofmaterials.
XRFanalyzersdeterminethechemistryofasamplebymeasuringthe
fluorescentX-rayemittedfromasamplewhenitisexcitedbyaprimaryX-ray
source.
Thephenomenoniswidelyusedforelementalanalysisandchemicalanalysis,
particularlyintheinvestigationofmetals,glass,ceramicsandbuildingmaterials,
andforresearchingeochemistry.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 81
X-RAY FLUORESCENCE

82. X-rayfluorescence(XRF)istheemissionofcharacteristic“secondary”(or
fluorescent)X-raysfromamaterialthathasbeenexcitedbybeingbombarded
withhigh-energyX-raysorgammarays.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 82
X-RAY FLUORESCENCE -PRINCIPLE

83. SourceofX-raysusedtoirradiatethesample.
Wavelengthsaretypicallyintherange0.01to10nm,whichisequivalentto
energiesof125keVto0.125keV.
DetectionequippedbyGas-filleddetectors,semiconductordetector,scintillation
detector,aphotographicplate.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 83
COMPONENTS OF A TYPICAL XRFSPECTROMETER

84. TheXRFspectroscopydiffersprimarilybydetectionandanalyzing.
(1)EnergyDispersiveXRF(Directandpolarizedexcitation)
(a)EnergyDispersiveX-rayfluorescencewithdirectexcitation
(b)EnergyDispersiveX-rayfluorescencewithpolarizedexcitation
(2)WavelengthDispersiveXRF
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 84
TYPES OF XRFSPECTROMETER

85. (a)EnergyDispersiveX-rayfluorescencewithdirectexcitation
Anenergydispersivedetectionsystemdirectlymeasuresthedifferent
energiesoftheemittedX-raysfromthesample.Bycountingandplottingthe
relativenumbersofX-raysateachenergyanXRFspectrumisgenerated.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 85

86. (b)EnergyDispersiveX-rayfluorescencewithpolarizedexcitation
Thedetectormustbeperpendiculartotheplanedeterminedbythetube,
targetandsample.ThemostimportanteffectisthatbydeflectingtheX-ray
radiationby90
o
,theradiationispolarizedandthespectralbackgroundinthe
spectrumisreduced.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 86

87. (2)WavelengthDispersiveX-rayfluorescence
TheX-raysaredirectedtoacrystal,whichdiffractstheX-raysindifferent
directionsaccordingtotheirwavelengths(energies).Onasequentialsystema
detectorisplacedatafixedposition,andthecrystalisrotatedsothatdifferent
wavelengthsarepickedupbythedetector.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 87

88. AsolidoraliquidsampleisirradiatedwithhighenergyX-raysfromacontrolled
X-raytube.
WhenanatominthesampleisstruckwithanX-rayofsufficientenergy,an
electronfromoneoftheatom’sinnerorbitalshellsisremoved.
Theatomregainsstability,fillingthevacancyleftintheinnerorbitalshellwith
anelectronfromoneoftheatom’shigherenergyorbitalshells.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 88
WORKINGOF X-RAY FLUORESCENCE

89. TheelectrondropstothelowerenergystatebyreleasingafluorescentX-rays.
TheenergyofthisX-raysisequaltothespecificdifferenceinenergybetween
twoquantumstatesoftheelectron.
ThemeasurementofthisenergyisthebasisofXRFanalysis.
Theintensityofeachcharacteristicradiationisdirectlyrelatedtotheamountof
eachelementinthematerial.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 89
WORKINGOF X-RAY FLUORESCENCE

90. •Itisamethodofelemental(metal&nonmetal)analysiswithatomicnumbergreater
than12.
•Quantitativeanalysiscanbecarriedoutbymeasuringtheintensityoffluorescenceat
thewavelengthcharacteristicsoftheelementbeingdetermined,especiallyapplicableto
mostoftheelementintheperiodictable.
•Researchinigneous,sedimentaryandmetamorphicpetrology,soilsurveys,mining(eg.,
measuringthegradeofore),cementproduction,ceramicandglassmanufacturing.
•Metallurgy(eg.,qualitycontrol)
•Environmentalstudies(eg.,analysesofparticulatematteronairfilters)
•Petroleumindustry(eg.,sulfurcontentofcrudeoilsandpetroleumproducts)
•Fieldanalysisingeologicalandenvironmentalstudies(usingportable,hand-heldXRF
spectrometers)
•Bulkchemicalanalysesofmajorelementsandtraceelements
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 90
APPLICATIONS

91. •Simple spectra analysis
•XRF is a versatile and rapid technique
•Easily analysis of the element among the same family elements
•It is non-destructive method of chemical analysis
•Important as in case of samples in limited amounts, or valuable or
irreplaceable
•It is precise and with skilled operations it is accurate
•Applicable to a wide variety of samples from powders to liquids
•It is convenient and economical to use
•Applicable over a wide range of concentrations.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 91
ADVANTAGES

92. •Itfairlyhighlimitsofdetectionwhencomparedtoothermethods
•Possibilityofmatrixeffects,althoughthesecanusuallybeaccountedfor
usingsoftware-basedcorrectionprocedures
•Itislimitedintheirabilitytopreciselyandaccuratelymeasuresthe
abundancesofelementswithatomicnumber<11inmostnaturalearth
materials.
•XRFanalysescannotdistinguishvariationsamongisotopesofanelement
•Instrumentationisfairlyexpensive
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 92
DISADVANTAGES

93. •ElementalAnalysisisaprocesswhereasampleofsomematerial(eg.Soil,waste
ordrinkingwater,bodilyfluids,minerals,chemicalcompounds)isanalyzedfor
itselementalandsometimesisotopiccomposition.
•Elementalanalysiscanbequalitative(determiningwhatelementsarepresent),
anditcanbequantitative(determininghowmuchofeacharepresent).
•Elementalanalysisfallswithintheambitofanalyticalchemistry,thesetof
instrumentsinvolvedindecipheringthechemicalnatureofourworld.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 93
ELEMENTAL ANALYSIS BY INDUCTIVELY COUPLED PLASMA

94. •CHNXanalysis
•Quantitativeanalysis
•Qualitativeanalysis
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 94
METHODS OF ELEMENTAL ANALYSIS

95. •Thedeterminationofthemassfractionsofcarbon,hydrogen,nitrogenand
heteroatoms(X)[halogens,sulfur]ofasample.
ThevariesCHNXanalysisare,
i)NMR(NuclearMagneticResonance)
ii)Massspectrometrychromatographic
iii)Combustionanalysis
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 95
1. CHNX analysis

96. •Quantitativeanalysisisthedeterminationofthemassofeachelementor
compoundpresent.Thequantitativeanalysisare,
i)Gravimeteryanalysis
ii)Opticalatomicspectroscopy(Flameatomicabsorption,Graphitefurnace
atomicabsorption,andInductivelycoupledplasmaatomicemission
spectroscopy)
iii)Neutronactivationanalysis
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 96
2. Quantitative analysis

97. •Toqualitativelydeterminewhichelementsexistsinasample
Massspectrometric(atomicspectroscopy)
Inductivelycoupledplasmamassspectrometry
X-rayfluorescence
Particle-inducedX-rayemission
X-rayphotoelectronspectroscopy
Augerelectronspectroscopy
Sodiumfusiontest
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 97
3. Qualitative analysis

98. •Theexcitationsourcemustdesolvate,atomize,andexcitetheanalyteatoms.
•Avarietyofexcitationsourcesareflame,arc/sparkandplasma.
PLASMA
•Plasmaisanelectricalconductinggaseousmixturecontainingsignificant
amountsofcationsandelectrons(netchargeapproacheszero)
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 98
EXCITING SOURCE OF MASS AND EMISSION SPECTROMETRY

99. •Increasedatomization/excitation
•Widerrangeofelements
•Simultaneousmultielementalanalysis
•Widedynamicrange
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 99
Advantages of PLASMA

100. •Direct-currentplasma(DCP)–InaDCP,aDCcurrentpassingbetweentwo
electrodesheatstheplasmagas,againtypicallyargon,andproducesadischarge.
Themostcommonversionisthethree-electrodesystem.
•Microwave-inducedplasma(MIP)–AMIPisanelectrodelessdischarge
generatedinaglassorquartzcapillarydischargetube,ofteninresonantcavity.
•CapacitivelyCoupledMicrowavePlasmas(CMP)–ACMPisformedusinga
magnetrontoproducemicrowaveenergyat2.45GHz.
•Inductively-coupledplasma(ICP)
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 100
TYPES OF PLASMA

101. •AnInductivelycoupledplasma(ICP)orTransformercoupledplasma(TCP)isatypepf
plasmasourceinwhichtheenergyissuppliedbyelectriccurrentswhichare
producedbyelectromagneticinduction,thatisbytime-varyingmagneticfields.
•Themostcommonlyusedionsourceforplasmaspectrometry,theICPisproducedby
flowinganinertgas,typicallyargon,throughawater-cooledinductioncoilwhichhas
ahigh-frequencyfield(typically27MHz)runningthroughit.
•Aninductivelycoupledplasma(ICP)isaveryhightemperature(7000-8000K)
excitationsources.ICPsourcesareusedtoexciteatomsforatomic-emissions
spectroscopyandtoionizeatomsformassspectrometry.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 101
INDUCTIVELY-COUPLED PLASMA (ICP)

102. •InductivelycoupleddischargealsousesRFpowersupplylikecapacitivelycoupled
discharge.
•Aradiofrequency(RF)generator(typically1-5kW@27MHx)producesanoscillating
currentinaninductioncoilthatwrapsaroundthetubes.
•Foracommonlyusedcylindricalplasmachambershownbelow,antennaisusually
wrappedaroundtheelectricallyinsulatingchamberwall.
•RFgeneratordriveshighalternatingcurrentthroughcoilantenna,whichcreatesan
alternatingmagneticfieldwithintheplasmachamber.
•Oscillatingmagneticfieldwillgenerateanoscillatingelectricfieldintheplasmachamber.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 102
PRODUCTION OF PLASMA

103. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 103
PRODUCTION PROCESS OF PLASMA

104. •Eventually,theelectricfieldwillacceleratetheelectronsandgenerateplasma.
•Themagneticfieldinturnsetsupanoscillatingcurrentintheionsandelectronsof
thesupportgas(argon).Astheionsandelectronscollidewithotheratomsinthe
supportgas.
•Sincetheexcitationforceisdeliveredthroughmagneticfield,inductivelycoupled
dischargeisalsocalled“H-discharge”.
•Forsomeapplications,itisdescribedas“electrodelessdischarge”becausethereis
nocathodeoranoderequiredforinductivelycoupleddischarge.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 104
PRODUCTION OF PLASMA

105. •Hightemperature(7000-8000K)
•Highelectrondensity(1014-1016cm)
•Appreciabledegreeofionizationformanyelements
•Simultaneousmulti-elementcapability(over70elementsincludingPandS)
•Lowbackgroundemissionandrelativelylowchemicalinterference
•Highstabilityleadingtoexcellentaccuracyandprecision
•Excellentdetectionlimitsformostelements(0.1-100ngmL-1)
•Widelineardynamicrange(LDR)[fourtosixordersofmagnitude]
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 105
CHARACTERISTICS OPTICALLY COUPLED PLASMA

106. •OpticalEmissionSpectroscopyorOESanalysis,isarapidmethodfordetermining
theelementalcompositionofavarietyofmetalsandalloys.
BasedonexcitationsourceOpticalEmissionSpectroscopyisclassifiedas,
•InductivelyCoupledOpticalEmissionSpectroscopy
•GlowDischargeOpticalEmissionSpectrometry(GD-OES)orGlowDischargeMS
(GD-MS)
•ArcsparkOpticalEmissionSpectroscopy
•Flameemissionspectroscopy
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 106
OPTICAL EMISSION SPECTROSCOPY

107. •TheInductivelyCoupledOpticalEmissionSpectroscopy(ICP-OES)analysis
methoduseshigh-frequencyinductivelycoupledplasmaasthelightsource,and
isdealfortheelementanalysisofsamplesolutions.
107
INDUCTIVELY COUPLED OPTICAL EMISSION SPECTROSCOPY
https://www.slideshare.net/ThirumalValavan2/

108. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 108
Flow diagram of ICP-OES

109. PRINCIPLE
•Whenplasmaenergyisgiventoananalysissamplefromoutside,thecomponent
elements(atoms)isexcited.Whentheexcitedatomsreturntolowenergy
position,emissionrays(spectrumrays)arereleasedandtheemissionraysthat
correspondtothephotonwavelengtharemeasured.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 109
INDUCTIVELY COUPLED OPTICAL EMISSION SPECTROSCOPY

110. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 110
Components of ICP-OES

111. •Sampleintroduction
•Productionofemission
•Collectionanddetectionofemission
•Signalprocessingandinstrumentcontrol
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 111
CONSTRUCTION

112. A)Nebulizer
B)Pump
C)Spraychambers
D)Drains
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 112
1. Sample Introduction

113. A)Torches
B)RadioFrequencyGenerators
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 113
2. Production of Emission

114. A)TransferOptics
B)WavelengthDispersiveDevices
C)Detectors
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 114
3. Collection and Detection of Emission

115. A)SignalProcessing
B)Computerandprocessors
C)Software
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 115
4. Signal Processing and Instrument Control

116. •Thefirststepinananalysisistopreparethesamplesandstandardsfor
introductiontotheICP.
•Thisstepdependsonthephysicalandchemicalcharacteristicsofthesamples
andformsimpledilutiontoacomplexseriesofchemicalreactionsandother
preparationsteps.
•Thenextstepintheanalysisconcernsthesampleintroductionmethodand
hardwaretobeused.
•FormostICP-OESanalyses,thestandardsampleintroductionsystemprovided
withtheinstrumentwillbesufficient.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 116
Working of ICP-OES

117. •Ininductivelycoupledplasma-opticalemissionspectrometry,thesampleis
usuallytransportedintotheinstrumentasastreamofliquidsample.
•Insidetheinstrument,theliquidiscoveredintoanaerosolthroughaprocess
knownasnebulization.
•Thesampleaerosolisthentransportedtotheplasmawhereitisdesolvated,
vaporized,atomized,andexcitedand/orionizedbythesample.
•Theexcitedatomsandionsemittheircharacteristicradiationwhichiscollected
byadevicethatsortstheradiationbywavelength.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 117
Working of ICP-OES

118. •Theradiationisdetectedandturnedintoelectronicsignalsthatareconverted
intoconcentrationinformationfortheanalyst.
•Thenextstepinthedevelopmentofananalysismethodologyistoprogramthe
instrument,usingthecomputersoftwareprovidedwiththeinstrument,to
performthedatacollectionandprocessingsteps.
•Todothis,decisionsmustbemadeconcerningtheoperatingconditions,
wavelengthselection,instrumentcalibration,emissionmeasurement,andthe
actualsampleanalysis.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 118
Working of ICP-OES

119. •Extremelyhighsensitivity
•Almostfullelementalcoveragewithoutneedforspecificexcitationsources
•Linearrangeofseveralordersofmagnitude
•Veryaccuratequantificationatlowconcentrations
•Highsamplethroughoutenablingtheefficientanalysisoflargebatches
•ComplementaryanalysistotechniqueslikeXRF
•Largedynamiclinearrange
•Lowchemicalandmatrixinterferenceeffects
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 119
Advantage of ICP-OES

120. •Cumbersomesamplepreparation
•Theneedtogeneratecalibrationcurvesfromsamplesassimilarinallrespects
asthesamplesunderinvestigation
•Initialprogressisoftentimeconsumingandtedious
•Relativelylonganalysistimes
•Themethodisinherentlydestructive
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 120
Disadvantage of ICP-OES

121. •Traceanalysisofenvironmentalsoilandwatersamples
•Assessmentofmetaloresformassbalancesandprocesscontrol
•BoronandLithiainglasses
•Forensicanalysis
•Metalreleasetestingoftableware
•Determinationoftoxic,traceandmajorconstituentsincoalandslags
•AnalysisoflowalloysteelsforAs,B,Bi,Ce,La,P,SnandTa;High-precision
determinationofSiinsteels.
•Determinationofcontaminantsinhigh-purityAl.
•Analysisofsuperconductingmaterialsfortrace.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 121
APPLICATIONS

122. •Inductivelycoupledplasmamassspectrometry(ICP-MS)isaninstrumental
analyticaltechniquebasedontheuseofahightemperatureionizationsource
(ICP)coupledtoamassspectrometer.
•Itisanelementalanalysistechnologycapableofdetectingmostoftheperiodic
tableofelementsatmilligramstonanogramlevelsperliter.
•Itisusedinavarietyofindustriesincluding,butnotlimitedto,environmental
monitoring,geochemicalanalysis,metallurgy,pharmaceuticalanalysisand
clinicalresearch.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 122
INDUCTIVELY COUPLED PLASMA MASS SPECTROSCOPY

123. •Itisatypeofmassspectrometrythatusesaninductivelycoupledplasmato
ionizethesample.Itatomizesthesampleandcreatesatomicandsmall
polyatomicions,whicharethendetected.
•Itisknownandusedforitsabilitytodetectmetalsandseveralnon-metalsin
liquidsamplesatverylowconcentrations.
•Itcandetectdifferentisotopesofthesameelement,whichmakesitaversatile
toolinisotopiclabeling.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 123
INDUCTIVELY COUPLED PLASMA MASS SPECTROSCOPY
PRINCIPLE

124. •Thisinternalstandardconsistsprimarilyofdeionizedwater,withnitricor
hydrochloricacid,andIndiumand/orGallium.
•Dependingonthesampletype,usually5mLoftheinternalstandardisaddedtoa
testtubealongwith10-500microlitersofsample.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 124
INDUCTIVELY COUPLED PLASMA MASS SPECTROSCOPY
SAMPLE PREPARATION

125. •Peristalticpump
•Nebulizerandspraychamber
•Torch
•PlasmaIonizationSource
•InterfaceRegion(Skimmercone&Samplercone)
•IonFocusingRegion
•Massanalyzer(Massspectroscopy)
•SpectralInterferences
•CollisionReactionCell(CRC)
•IonDetectors
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 125
ICP-MS : COMPONENTS

126. •Tobeprocessesefficientlyintheplasma,samplesmustbeineithergasorvapor
(aerosol)form.
•So,whilegasescanbeanalyzeddirectlybytheplasma(eg.,whenseparatedby
gaschromatography),solidsandliquidshavetobeconvertedtoaerosolfrom
usingeitheranebulizer(forliquids)oranablationdevice(forsolids).
•Onlyasmallamountpartoftheionsproducedintheplasmafurtherpenetrateto
themass-spectrometerpart.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 126
WORKING OF ICP-MS

127. •Aftermassseparation,ionsmustbedetectedandamplifiedinorderto
determinetheirintensities.
•Electronmultipliersalsoknownassecondaryelectronmultiplier,orSEM
detector)candetectextremelysmallioncurrents,includingevensingleions,
comingfromthemassanalyzer.
•Theyoperateontheprincipleofsecondaryelectronemission,inwhichcharged
particleswithsufficientenergyincidentona“dynode”stimulatetheemissionof
electronsfromthesurface.
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WORKING OF ICP-MS

128. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 128
Working flow of ICP-MS

129. @ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 129
Working flow of ICP-MS

130. •Pumptubinghasthetendencytostretch,whichchangestheamountof
samplebeingdeliveredtothenebulizer.
•Tipofthenebulizershouldnotgetblocked.
•Microscopicparticlescanbuildonthetipofthenebulizerwithoutthe
operatornoticing,whichovertime,cancausealossofsensitivity,imprecision,
andpoorlong-termstability.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 130
MAINTENANCE OF ICP-MS

131. •Drainofspraychambermustfunctionproperly.Malfunctioningorleaking
draincanproducechangesinthespraychamberbackpressure,producing
fluctuationsintheanalytesignal,resultinginerraticandimprecisedata.
•Staininganddiscolorationoftheoutertubeofthequartztorchbecauseof
heatandthecorrosivenessoftheliquidsamplecancauseelectricalarcing.
•Themostcommontypesofproblemsassociatedwiththeinterfaceare
blockingorcorrosionofthesamplercone&skimmercone.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 131
MAINTENANCE OF ICP-MS

132. •Simplemetalanalysisduringmetalbaseddrugdevelopment
•Impuritylimittests
•Metalspresentinactivepharmaceuticalingredients
•Monitoringmetabolitesofanadministereddrug
•Detectionofmetalimpuritiesfromleachablepackingmaterial
•Forelementalspeciation
•Pharmaceuticalwastewatermonitoring.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 132
Application of ICP-MS

133. •Quantitativeanalysisisthefundamentaltoolusedtodetermineanalyteconcentrations
inunknownsamples.
•Increasedsensitivelyandwidedynamicrange
•Extremelylowdetectionlimits
•Alargelinearrange
•Wideelementalcoverage
•Simplespectra
•Isotopicinformation
•Highthroughput&Productivity
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 133
Advantage of ICP-MS

134. •Thehighcapitalcostoftheinstrumentation
•Lowerprecisioncomparedwithatomicabsorptionsspectrometry(AAS)
•Thetotaldissolvedsaltsshouldbelessthan1000ppm
•Severematrixeffects
•Heavierelements,suchaslead,arewell-suitedforICP-MSanalysis,whereas
lighterelementsarepronetomoreinterference.
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC. 134
Disadvantage of ICP-MS

135. THANK YOU
135
©S.Thirumalvalavan, Assistant Professor,
Department of Mechanical Engineering,
E-Mail : [email protected]
@ S. Thirumalvalavan, AP/Mech, 5104 -AEC.
https://www.slideshare.net/ThirumalValavan2/