XraydiffractionanalvsesofCdS(XRD)MicrowavesyntheticrouteSinglesourceprecursormethodologyTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTTT0CdSQDsCdSQDs(TTT)00(zz)(OL)(cOL)(TEE(Z1)(Z)(()N278°C12T=225°CT=225°CT=178°℃3040506020307080207010405060902020HexagonalstructureCubic StructureWurtzitephaseJune2014CNEM&T
June 2014 ICNEM&T 26 Hexagonal structure Würtzite phase Single source precursor methodology Microwave synthetic route Cubic Structure(111) (220) (331) (331) & (420) (442) (551) X ray diffraction analyses of CdS (XRD)
Then....why using mass spectrometry??Investigationinorganic,inorganic,organometalliccompounds,polymers1-lonizationtechniqueatomicm/zmolecular2-Massspectrometersystemm/△mstructuralQuad,TripleQuad,ToF,QTof,lonTrap,,FTICRMS,Orbitrap,et...PrecursorsNanomaterialsAvailabledata!!Synthesis stepsJune2014ICNEM&T27
June 2014 ICNEM&T 27 Then.why using mass spectrometry?? Investigation in organic, inorganic, organometallic compounds, polymers 1 - Ionization technique 2 - Mass spectrometer system Quad, TripleQuad, ToF, QTof, Ion Trap, , FTICRMS, Orbitrap, etc. atomic molecular structural Available data!! Precursors Nanomaterials Synthesis steps m/z m/Dm
Massspectrometry??Measuring molecules weight with a high accuracy!!!You need:lonizedatoms ormoleculesinthegas phaseSeparation withananalyserratio m/zismeasuredfortheseionsm/zamu or Dalton1u=1Da=1,66053886x10-27kgJune201428ICNEM&T
Mass spectrometry ?? Measuring molecules weight with a high accuracy!!! You need: Ionized atoms or molecules in the gas phase Separation with an analyser ratio m/z is measured for these ions amu or Dalton 1 u = 1 Da = 1,66053886 x 10-27 kg m / z June 2014 28 ICNEM&T
Majorcomponentsof massspectrometerFixedgases oryolatile liguidsbyEl,Cl,orFlSolids orsolutionsDetectorlonSourcem/zAnalyzerbyESI,APCIIONSIONSAP-MALDIVacuumSolidsbyMALDIorLSIMSComputerldatasystemJune2014ICNEM&T29
Major components of mass spectrometer Ion Source Solids by MALDI or LSIMS Solids or solutions by ESI, APCI, AP-MALDI Fixed gases or volatile liquids by EI, CI, or FI IONS m/z Analyzer IONS Detector Computer/data system Vacuum June 2014 ICNEM&T 29
Gas-phaseionizationofanalytesfollowedbyionseparationaccordingtothem/zvaluelonizationm/z29m/z27MMMM+.MM+MMM.MMMMMM*-MM*MMMMMMMMM*-M+.1294358MMM+MMMMMMMMMMM+MM+massspectrumm/z57m/z43m/z15omassanalysisofallionsionization andsamplevaporuni-molecularabsorptionofexcessdata recordingmol.mass58decompositionofM+energyplot of bar graphICNEM&T30June2014
Gas-phase ionization of analytes followed by ion separation according to the m/z value M M M M M M M M M M M M M M M M M M M M M M M M. M M M M M+- M+. M M M M+ M M M M+- M+- M+ M+- M M+ M+- Ionization sample vapor mol. mass 58 ionization and absorption of excess energy uni-molecular decomposition of M+. mass spectrum 29 43 58 m/z 29 m/z 27 m/z 57 m/z 15 m/z 43 ° mass analysis of all ions ° data recording ° plot of bar graph June 2014 ICNEM&T 30