Microwaves in organic synthesis Vol. 2

166 Pages·2009·1.318 MB·English

by  J. Capelo-Martinez

Ultrasound in Chemistry
Edited by
Jos´e-Luis Capelo-Mart´ınez
Further Reading
Loupy,A.
Microwaves in Organic Synthesis
Second,CompletelyRevisedandEnlargedEdition
2006
Hardcover
ISBN:978-3-527-31452-2
Kappe, C. O.,Dallinger,D., Murphree, S.S.
Practical Microwave Synthesis for Organic Chemists
Strategies,Instruments,andProtocols
2009
Hardcover
ISBN:978-3-527-32097-4
Koch,M. V.,VandenBusche, K. M.,Chrisman, R.M.
Microinstrumentation
forHighThroughputExperimentationandProcessIntensification
2007
Hardcover
ISBN:978-3-527-31425-6
Kromidas, S.,Kuss, H.-J.
Quantification in LC and GC
APracticalGuidetoGoodChromatographicData
2009
Hardcover
ISBN:978-3-527-32301-2
Ultrasound in Chemistry
Analytical Applications
Edited by
José-Luis Capelo-Martínez
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ISBN:978-3-527-31934-3
V
Contents
Preface XI
List of Contributors XIII
1 ThePowerofUltrasound 1
HugoMiguelSantos,CarlosLodeiro,andJosé-LuisCapelo-Martínez
1.1 Introduction 1
1.2 Cavitation 1
1.2.1 ParametersAffectingUltrasonicCavitation 3
1.2.1.1 Frequency 3
1.2.1.2 Intensity 4
1.2.1.3 Solvent 5
1.2.1.4 Temperature 5
1.2.1.5 ExternalPressureandBubbledGas 5
1.2.1.6 DirectandIndirectUltrasonicApplication 6
1.3 CommonUltrasonicDevicesUsedinAnalyticalChemistry 6
1.3.1 UltrasonicBath 6
1.3.1.1 TypesofUltrasonicBaths 7
1.3.1.2 HowtoLocatetheMostEfficientPlaceInsideanUltrasonicBath 8
1.3.1.3 TemperatureControl 8
1.3.1.4 ShapeandMaterialofReactionContainer 9
1.3.2 TheUltrasonicProbe 9
1.3.2.1 PartsofanUltrasonicProbe 10
1.3.2.2 TypesofUltrasonicProbes 10
1.3.2.3 DeadZones 11
1.3.2.4 HowtoChoosetheCorrectUltrasonicProbe 12
1.3.2.5 TemperatureControl 13
1.3.2.6 ShapeandMaterialofReactionContainer 14
1.4 CurrentUltrasonicDevicesforNewAnalyticalApplications 14
References 15
UltrasoundinChemistry:AnalyticalApplications.EditedbyJosé-LuisCapelo-Martínez
Copyright(cid:1)2009WILEY-VCHVerlagGmbH&Co.KGaA,Weinheim
ISBN:978-3-527-31934-3
VI Contents
2 UltrasonicEnergyasaToolforSampleTreatmentfortheAnalysis
ofElementsandElementalSpeciation 17
HugoMiguelSantos,CarlosLodeiro,andJosé-LuisCapelo-Martínez
2.1 Introduction 17
2.2 ParametersInfluencingElementUltrasonicSolid–Liquid
Extraction 17
2.2.1 ExtractingReagent 17
2.2.1.1 ExtractingReagentsforTotalElementExtraction 18
2.2.1.2 ExtractingReagentsforElementalSpeciation 19
2.2.1.3 ExtractingReagentsforSequentialExtractionSchemes 19
2.2.2 MatrixProperties 20
2.2.2.1 TypeofMatrix 20
2.2.2.2 MassofMatrix 20
2.2.2.3 SampleSize 22
2.2.3 UltrasonicDevice 22
2.2.3.1 TypeofUltrasonicDevice 22
2.2.3.2 TimeofUltrasonication 23
2.2.3.3 UltrasonicAmplitude 23
2.2.3.4 UltrasonicFrequency 23
2.2.3.5 TemperatureofSonication 23
2.3 US-SLEfromSoilsandSediments 24
2.4 US-SLEfromSewageSludge 24
2.5 US-SLEExtractionfromPlants 24
2.6 ExtractionfromSoftTissues 27
2.7 TotalElementDetermination 27
2.7.1 US-SLEandUS-SSforF-AAS 27
2.7.2 US-SLEandUS-SSforET-AAS 28
2.7.3 US-SLEandUS-SSforCVandHGEmployedwith
AASorAFS 28
2.8 ElementalFractionationandElementalSpeciation 30
2.8.1 WhatisSpeciation? 30
2.8.2 ShorteningSequentialFractionationSchemes 31
2.8.3 SpeciationforSoilsandSediments 34
2.8.4 SpeciationfromPlants 34
2.8.5 SpeciationfromSoftTissues 36
2.8.6 SpeciationfromOtherTypesofSamples 43
2.9 On-LineApplications 45
2.9.1 OpenandClosedSystems 46
2.9.2 UB 47
2.9.3 UP 47
2.10 CurrentTrends 48
2.10.1 AcceleratingLiquid–LiquidExtractions 48
2.10.2 ChemicalVaporFormation 49
2.11 Conclusion 49
References 50
Contents VII
3 UltrasonicAssistedExtractionfortheAnalysisofOrganicCompounds
byChromatographicTechniques 55
RaquelRial-Otero
3.1 Introduction 55
3.2 OverviewofClassicandModernExtractionProceduresforOrganics 56
3.3 UltrasonicAssistedExtraction(UAE) 60
3.3.1 BasicPrinciples 60
3.3.2 ParametersInfluencingUltrasonicAssistedExtraction 61
3.3.2.1 AmountofSample 61
3.3.2.2 SampleParticleSize 61
3.3.2.3 ExtractionSolvent 61
3.3.2.4 pHofExtractingSolution 62
3.3.2.5 SolventVolume 62
3.3.2.6 SonicPower 62
3.3.2.7 Frequency 63
3.3.2.8 ExtractionTime 63
3.3.2.9 ExtractionTemperature 63
3.3.3 Applications 63
3.3.3.1 LiquidSamples 64
3.3.3.2 SolidSamples 64
3.3.3.3 Clean-Up 70
3.4 CouplingUltrasoundwithOtherExtractionTechniques 71
3.4.1 CouplingSolidPhaseMicroextraction(SPME)andUltrasound 71
3.4.1.1 ImprovingtheExtractionProcedureinDirect-SPME 71
3.4.1.2 ImprovingtheExtractionProcedureinHS-SPME 73
3.4.1.3 FacilitatingtheDesorptionProcess 73
3.4.2 CouplingStirBarSorptiveExtraction(SBSE)andUltrasound 74
3.5 ComparisonbetweenUAEandOtherExtractionTechniques 75
3.6 Conclusion 76
References 77
4 ElectrochemicalApplicationsofPowerUltrasound 81
NeilVaughanReesandRichardGuyCompton
4.1 Introduction 81
4.2 ElectrochemicalCellandExperimentalSetup 87
4.3 VoltammetryUnderInsonation 87
4.4 TraceDetectionbyStrippingVoltammetry 88
4.4.1 ClassicalElectroanalysis 89
4.4.2 ElectroanalysisFacilitatedbyUltrasound 90
4.4.3 ApplicationsofSono-AnodicStrippingVoltammetry(Sono-ASV) 90
4.5 BiphasicSonoelectroanalysis 90
4.5.1 DeterminationofLeadinPetrol 90
4.5.2 ExtractionandDeterminationofVanillin 92
4.5.3 DetectionofCopperinBlood 92
4.6 MicroelectrodesandUltrasound 93
VIII Contents
4.6.1 InsightsintoBubbleDynamics 93
4.6.2 MeasurementofPotentialsofZeroCharge(PZC) 95
4.6.3 ParticleImpactExperiments 96
4.7 Conclusion 102
References 103
5 PowerUltrasoundMeetsProtemics 107
HugoMiguelSantos,CarlosLodeiro,andJosé-LuisCapelo-Martínez
5.1 Introduction 107
5.2 ProteinIdentificationthroughMass-BasedSpectrometryTechniques
andPeptideMassFingerprint 108
5.3 ClassicIn-GelProteinSampleTreatmentforProteinIdentification
throughPeptideMassFingerprint 108
5.4 UltrasonicEnergyfortheAccelerationofIn-GelProteinSample
TreatmentforProteinIdentificationthroughPeptideMass
Fingerprint 111
5.4.1 Washing,ReductionandAlkylationSteps 111
5.4.2 In-GelProteinDigestionProcess 113
5.4.2.1 SampleHandling 113
5.4.2.2 SonicationVolume 115
5.4.2.3 SonicationTime 115
5.4.2.4 SonicationAmplitude 115
5.4.2.5 ProteintoTrypsinRatio 115
5.4.2.6 Temperature 116
5.4.2.7 Solvent 116
5.4.2.8 MinimumAmountofProteinIdentified 116
5.4.2.9 ReductionandAlkylationSteps 117
5.4.2.10 ComparisonwithOtherTypesofRapidSampleTreatments 117
5.4.2.11 InfluenceofProteinStaining 117
5.5 ClassicIn-SolutionProteinSampleTreatmentforProteinIdentification
throughPeptideMassFingerprint 118
5.6 UltrasonicEnergyfortheAccelerationoftheIn-SolutionProtein
SampleTreatmentforProteinIdentificationthroughPeptide
MassFingerprint 121
5.6.1 In-SolutionProteinDenaturation 121
5.6.2 In-SolutionProteinReductionandAlkylation 122
5.6.3 In-SolutionProteinDigestion 124
5.6.4 CleanIn-SolutionProteinDigestion 124
5.7 Conclusion 125
References 126
6 BeyondAnalyticalChemistry 129
CarlosLodeiroandJosé-LuisCapelo-Martínez
6.1 Introduction 129
6.2 SonochemistryforOrganicSynthesis 129
Contents IX
6.3 UltrasonicEnhancedSynthesisofInorganicNanomaterials 137
6.4 SonochemistryAppliedtoPolymerScience 139
6.4.1 IntroductiontoPolymers 139
6.4.2 UltrasonicationinSampleTreatmentforPolymer
Characterization 140
6.4.2.1 IntroductiontoPolymerCharacterization 140
6.4.2.2 OverviewofSamplePreparationforMALDIAnalysisofPolymers 141
6.4.2.3 UltrasonicEnergyasaToolforFastSampleTreatmentforthe
CharacterizationofPolymersbyMALDI 142
6.4.3 Ultrasonic-InducedPolymerDegradationforPolymer
Characterization 145
6.4.4 UltrasonicationforthePreparationofImprintedPolymers 145
6.5 Conclusion 148
References 148
Index 151