Instrumental Analysis

Robert M. Granger II is Chair and Professor of Chemistry at Sweet Briar College. Hank M. Yochum is Professor of Physics and Engineering and Director of the Margaret Jones Wyllie '45 Engineering Program at Sweet Briar College. Jill N. Granger is Dean of the Honors College at Western Carolina University. Karl D. Sienerth is Chair and Professor of Chemistry at Elon University.

• CHAPTER 1 - The Analyst's ToolboxProfile - A Scenario1.2 - Introduction1.2 - Ultraviolet - visible Spectroscopy1.3 - Infrared SpectroscopyCompare and Contrast - UV-vis vs. FTIR in Quantitative Analysis1.4 - Nuclear Magnetic Resonance Spectrometry1.5 - Mass SpectrometryProfile - Putting it All Together1.6 - ChromatographyProfile - Establishing a Forensic Protocol1.7 - Further Reading1.8 - Additional ExercisesCHAPTER 2 - Quantum Mechanics and SpectroscopyProfile- The Brain Initiative and everyday spectroscopy2.1- Introduction2.2- The interaction between electromagnetic radiation and matter - absorption and emission of lightProfile - Erwin Schrödinger2.3- Molecular vibrations lead to quantized energy levelsProfile - London's Millennium BridgeProfile- Mass Dampers2.4- Molecular rotation leads to quantized energy levels2.5- Transitions between vibrational and rotational states -the role of thermal energy and nonradiative decayPrelude - The Boltzmann Distribution2.6- Transitions between electronic, vibrational, and rotational states - putting it all togetherThe Jablonski diagramFluorescence and Phosphorescence2.7 Energy levels of a proton in a magnetic field - Nuclear Magnetic Resonance (NMR) Spectroscopy2.8- Additional ExercisesCHAPTER 3 - An Introduction to OpticsProfile: The diffraction grating is a key component for many optical instruments3.1 - An Introduction to the Properties of LightWavelength, Energy, and FrequencyCoherencePolarizationInterferenceDiffractionScatteringProfile- The photoelectric effect shows the particle nature of light3.2- Controlling optical beamsMirrors and ReflectionLenses and RefractionCollecting and Collimating LightFocusing a Collimated Laser BeamPolarizers3.3- Wavelength Selection Introduction to Prism and Grating MonochromatorsThe Diffraction GratingPutting it all together- Details on the Grating Monochromator Profile- Optics that operate by diffraction- the Fresnel Zone PlateThe Michelson InterferometerOptical Filters & Power Reduction3.4 - Common Optical Materials3.5- Beyond Linear OpticsProfile- Innovation and discovery in optics - metamaterials hold promise for the perfect lens, invisibility cloaks, and more3.6- Further Reading3.7 - Additional ExercisesCHAPTER 4 - An Introduction to Instrumental Electronics4.1 - IntroductionCircuit Symbols4.2 - DC CircuitsCurrent, Voltage, and Multimeter BasicsSeries Circuit Elements and the Voltage DividerParallel Circuit Elements and the Current DividerThe Multimeter Voltage and Current Loading ErrorProfile - Electronics for a Very Simple Light Sensing Instrument: Voltage Divider Photoresistor circuit 4.3- Capacitors and RC Circuits4.4- AC CircuitsOhm's law for AC circuitsLow-pass, High-pass, Band-pass, and Band Stop FiltersActivity- RC Filter Spreadsheet Tool4.5 - Operational Amplifiers Inverting and Non-inverting op ampsSumming op ampCurrent to Voltage AmplifierThe Voltage FollowerOp Amp ComparatorCascading op amps A Cascaded Op Amp Example- Instrumentation Op AmpProfile- Electronics for an Automatic Titrator: Cascaded Op Amps and the Differentiating Op Amp 4.6 - Quick Survey of ComponentsPotentiometersDiodeTransistorsProfile- Electronics for a Simple Absorption Spectrophotometer: Op Amp Circuit as Current to Voltage AmplifierProfile- What if you need a constant voltage under varying loads? A basic schematic of a potentiostat4.7 - Analog and Digital Signals4.8 - Further Reading4.9 - Additional ExercisesCHAPTER 5 - Signals and Noise: An Introduction to Signal ProcessingProfile- Spectroscopy of single molecules?5.1 - Introduction to Signals5.2 - Sources and Characteristics of Noise5.3 - Signal to Noise Ratio and Ensemble Averaging5.4- Processing Signals with Hardware and SoftwareAnalog Filters Boxcar averaging with hardwareModulating Signals and the Lock-In AmplifierDigital FiltersRolling average, Boxcar average, Savitzky-Golay Filter, and Fourier Filtering5.5 - Sampling Rates, the Nyquist Frequency, and Aliasing5.6- Analog to Digital Conversion5.7- Further Reading5.8 - Additional ExercisesCHAPTER 6 - Molecular Ultraviolet and Visible Spectroscopy. Profile - James Clerk Maxwell6.1 - Introduction6.2 - Electronic Excitation and Molecular StructureStructure and "Color" HeteroatomsDPK - A Case StudySolvent PolarityTransition Metal Coordination Compounds Vibronic TransitionsSidebar - The Spectroscopic Series6.3 - Quantitative MeasurementsSelection RulesBeer's LawSidebar - Derivation of Beer's LawDeviations from Beer's LawBandwidth ResolutionActivity - Explore the effects on the relationship of A vs. c6.4 - Instrumentation DesignsFixed Wavelength SpectrometersProfile - HACH DR3900Scanning SpectrometersCompare and Constrast - Single & Dual Beam SpectrometersArray Spectrophotometers6.5 - Monochromators6.6 - SourcesDeuterium Arc/Tungsten Halogen BulbXenon Arc LampsLight Emitting DiodesProfile - The Jaz® by Ocean Optics6.7 - DetectorsThe PMTPhotovoltaic CellsCharge Coupled Device 6.8 - Noise Stray LightDetector NoiseProfile - Walter Hermann SchottkySource Noise6.9 - Kinetic UV-vis TechniquesStop Flow UV-visFlash PhotolysisProfile - Building a functional monochromator6.10 - Useful Data6.11 - Further Reading6.12 - Additional ExercisesCHAPTER 7 - Atomic Absorption Spectroscopy 7.1- IntroductionProfile - The Birth of Atomic Absorption Spectroscopy (AAS)7.2 - Molecular vs. Atomic AbsorptionAnalytical Specificity7.3 - Spectral BandwidthLifetime BroadeningProfile - Review of Term SymbolsMagnetic Field BroadeningProfile - Lightning over Salty WatersPressure BroadeningNote - IUPAC nomenclature for pressure broadening.Doppler Broadening7.4 -AAS SourcesThe Hollow-Cathode LampProfile - Nutritional Contents of Breast MilkElectrodeless Discharge LampsActivity - Soil Analysis7.5 - Sample IntroductionFlame - AASThe FlameThe Flame HeightElectrothermal-AAS/GFAASFlame vs Electrothermal AASProfile- AAS Analysis of OilHydride - AASCold Vapor-AASCompare and Contrast - Detection Limit Ranges7.6 - Measuring Atomic AbsorptionBackground CorrectionZeeman Background CorrectionSmith-Hieftje background correction Spectral InterferenceProfile-Demystifying the Zeeman Effect7.7 - Sample PreparationAcid Digestion7.8 - Performing an AAS analysis7.9 - Further Reading7.10 - Additional ExercisesCHAPTER 8 - Luminescence Spectroscopy8.1 - Introduction 8.2 - TheoryPrinciples of Fluorescence and PhosphorescenceProfile - Is your $100 bill real? Find out with time-resolved fluorescenceRelating fluorescence and molecular structure Profile - Fluorescence quenching helps with aerodynamics8.3 -The Fluorescence SpectrometerExcitation sourcesWavelength discrimination and instrument resolutionDetectorsPutting it all together- Walking through the luminescence systemExcitation spectraSample introductionProfile- Fluorescence pushes the limits of detection- single molecule detection and femtomolar concentrations8.4- Challenges with Fluorescence SpectroscopyDetector response correctionSource intensity correctionStray light contaminationChallenges with high absorbancePhotobleaching8.5 -Additional Fluorescence based techniquesChemiluminescenceFluorescence polarizationResonance energy transfer spectroscopyMultiphoton excitation8.6 -Further Reading8.7 - Additional ExercisesProfile - Using fluorescence to determine concentrations of DNA and RNACHAPTER 9 - Atomic Emission Spectroscopy9.1 - IntroductionProfile - Get The Lead Out9.2 - The Atomizer and the Excitation SourceProfile - ColumbiaInductively Coupled Plasma Torch Direct Current Plasma SourceProfile - The Plasma TorchMicrowave Induced Plasma SourceProfile - Atmospheric MP-AESProfile - LIBS in SpaceLaser AblationProfile- Visualizing a Plasma9.3 - Sample IntroductionApplicationsSources AAS vs. AESSample preparation and interferencesZeeman Background Correction9.4 - Measuring Atomic EmissionCompare and Contrast FAAS, GFAAS & ICP-AES9.5 -Further Reading9.6- Additional ExercisesCHAPTER 10 -X-Ray Related TechniquesProfile - A modern day gold rush. 10.1- Principles of X-ray Fluorescence (XRF) Profile-W. C. RöntgenXRF Transitions: TerminologyPhotoelectric AbsorptionCompare and Contrast - Optical Absorption vs.Photoelectric AbsorptionAbsorption of X-rays10.2- X-ray SourcesRadioisotopesX-ray tubesSynchrotron RadiationProfile -Lost Inscriptions10.3- X-ray Optics Profile -XRF Analysis of a 15th PaintingReflection OpticsDiffraction OpticsProfile - Lost Painting by Vincent van Gogh10.4- Wavelength Dispersive Spectrometers Sequential and SimultaneousWDXRF Detectors10.5- Energy Dispersive SpectrometersEDXRF Detectors10.6- Direct Comparison: WDXRF & EDXRFCompare and Contrast- AAS, AES & XRF10.7- Sample Introduction10.8- Total Reflection XRF (TXRF)Profile - Christiaan HuygensProfile- Max Von Laue10.9- X-ray Induced Photoelectron Spectroscopy & Auger Electron SpectroscopyCompare and Contrast: XRF, XPS & AES XPSAESProfile - Pierre Victor AugerXPS & AES Instrumentation10.10- Single Crystal X-ray DiffractometryScatterX-ray DiffractionBragg's LawProfile- Henry and Lawrence BraggThe LatticeObtaining A Crystal StructureThe Diffractometer10.10- Further Reading10.11- Additional Exercises Advanced ExercisesCHAPTER 11 -Infrared Spectroscopy11.1 -Chemical Structure and Molecular VibrationsProfile - The Future of FTIRWavenumbersGroup FrequenciesNormal ModesVibrational CategoriesProfile - Olive OilThe Selection Rules and Molecular SymmetryVibronic Coupling11.2 - Time Domain vs. Frequency Domain Spectroscopy: The Fourier TransformationActivity: Creating a Beat PatternActivity: Performing a Fourier Transform 11.3 -FTIR & Wavelength Discrimination The Michelson Interferometer ResolutionActivity: Exploring Resolution 11.4 -SourcesThe Nernst GlowerThe GlobarCoiled Wire SourcesSolid State Sources11.5 -DetectorsThermal DetectorsPyroelectric DetectorsProfile- PZT CeramicsPhotoconductive DetectorsProfile- MCT DetectorsQuantum Well Detectors11.6 -Spectral OutputTransmittance vs. AbsorbanceQuantitative Measurements and Deviations from Beer's Law11.7- Developments; Two Dimensional Infrared Spectroscopy11.8 - Sample IntroductionOptical MaterialsGassesSolution IR SpectroscopyNeat LiquidsSolidsATRCompare and Contrast: UV-vis versus FTIR in Quantitative & Qualitative Analysis11.9 - Useful Data11.10 - Further Reading11.11- Additional ExercisesCHAPTER 12 - Raman SpectroscopyProfile - Raman Applications in Art and Medicine12.1 -IntroductionRayleigh Scattering12.2 - Theory of Raman ScatteringSelection RulesCase Study - Vibrations in the linear molecule CO2Case Study- Raman spectroscopy of a tetrahedral molecule; CCl412.3 -The Raman SpectrometerInstrument BasicsRadiant SourceWavelength Discrimination and RamanSpectrometer ResolutionFiltersDetectorsCompare and Contrast - A side-by-side evaluation of FTIR and Raman spectroscopy.Handheld Raman Analyzers Profile - Drug detection using commercial handheld Raman spectrometersFiber optic probes12.4- Additional Raman based techniquesRaman ImagingPolarized Raman SpectroscopyFourier Transform Raman Spectroscopy (FT-Raman)Surface enhanced Raman Spectroscopy (SERS)Profile - Using Raman spectroscopy to identify compounds from a distance12.5 - Further Reading12.6 - Additional ExercisesCHAPTER 13 - Mass Spectrometry13.1 - Basic Principles & Comparisons to an Optical SpectrophotometerProfile - Puffer MS13.2 - Ion sourcesElectron IonizationProfile - J. J. ThomsonChemical IonizationElectrospray IonizationProfile - John FennMatrix Assisted Laser Desorption IonizationSecondary Ion Thermal IonizationInductively Coupled PlasmaCompare & Contrast - Elemental MethodsProfile - TOF-MS in Space13.3 - Mass AnalyzersSector & Double-focusingProfile - Eugen Goldstein QuadrupoleProfile - R. Graham CooksTime-of-flightFT Ion Cyclotron Resonance13.4 - DetectorsActivity - Selected Ion Game13.5 - Additional TechniquesTandem TechniquesIsotope Ratio Mass SpectrometryAccelerator Mass SpectrometryProfile - 10Be as a Geological ClockProfile - Human Scent Fingerprinting13.6 - Further Reading13.7 - Additional ExercisesAdvanced ExercisesCHAPTER 14 - An Introduction to Nuclear Magnetic Resonance Spectroscopy14.1 - IntroductionProfile - NMR versus HIVSpectral Analysis - A Quick Review14.2 - NMR Spectroscopy is all about the NucleusNuclear Quantum NumbersA Nucleus in a Magnetic FieldTesla vs. MHz14.3 - The NMR SignalCompare and Contrast - Population distribution for common spectroscopic methodsProfile - Felix Bloch14.4 - The RF Pulse: Inducing nuclear magnetic resonanceFT-NMR: Time Domain vs. Frequency Domain Spectroscopy & The Fourier TransformationFree Induction Decay (FID): The FT-NMR "Beat Pattern"14.5 - Chemical Shift and ResolutionProfile - Richard R. ErnstThe Chemical Shift (ppm)Chemical Shift ReferenceResolution14.6 - The Instrument ShimmingLoading14.7 - Signal Processing Increasing the signal to noise ratioProfile - Angela Gronenborn14.8 - Magnetic Resonance ImagingProfile - MRI and Brain Concussion14.9 - Further ReadingTextsOn Line ResourcesSome interesting laboratory experiments14.10 - Additional ExercisesCHAPTER 15 - Liquid Chromatography15.1 - IntroductionProfile- Mikhail S. Tswett15.2 - TheoryDistribution EquilibriumProfile - Other Applications of Partition CoefficientsPrinciples of ChromatographyActivity: TLC at homeThe Retention FactorResolution and Theoretical PlatesBand Broadening15.3 - Basic Method DevelopmentThermodynamics and Kinetics FactorsIsocratic vs. GradientProfile: The Role of TemperatureQualitative vs. Quantitative Profile: Analysis of Wine - Qualitative and Quantitative15.4 - Stationary Phase Materials and Modes of SeparationProfile: LC-MS in Athletic DopingNormal PhaseReversed PhaseIon ExchangeHydrophilic Interaction Chromatography (HIC)Affinity Chiral ChromatographyProfile - The Chiral Medicine CabinetSize Exclusion15.5 - InstrumentationOverview HPLC ComponentsProfile -Ultrahigh Pressure LCMobile PhaseColumns InjectorsPumpsDetectors Profile- Major Players, the Chromatography Industry15.7 - Further Reading15.8 - Additional ExercisesCHAPTER 16 - Gas ChromatographyProfile - Odorants, Pheromones, and Chemosignals16.1 - IntroductionProfile - Gas Chromatography on Mars16.2 - Basic GC Instrument Design16.3 - Method Development: a case studyA Case Study - Peanut ButterProfile - The NIST 14 Gas Chromatography (GC) Library with Search Software16.4 - Modes of SeparationIsothermal vs. Temperature gradientsThe Column16.5 - Carrier Gas and InjectorCarrier Gases16.6 - DetectorsIonizing DetectorsOptical Detectors Thermal Conductivity DetectorsElectrochemical Detectors Tandem Instrument DetectionQuantitative and Qualitative Considerations16.7 - New Developments and Directions in GCMultidimensional GC Techniques Profile - Breath and Air QualityMiniaturization, Portability, Speed, and Throughput16.8 - Extended TheoryEvaluation of the GC SeparationThe Relationship between VN, k, and SelectivityThe General Elution Problem16.9 - Useful InformationTable 16.3 - GC column Manufacturers16.10 - Further Reading16.11 - Additional ExercisesCHAPTER 17 - Electrophoresis17.1 - IntroductionProfile - The Father of Electrophoresis17.2 - Fundamental Principles17.3 - The Basic ApparatusProfile - DNA Markers17.4 - Paper Electrophoresis Activity -Demystifying Electrophoresis: Build Your Own Electrophoresis Apparatus17.5 - Gel ElectrophoresisPolyacrylamide Gel Electrophoresis (PAGE) SDS PAGEAgarose Gel Electrophoresis17.6 - Ending the Analysis: The Time Factor17.7 - Gel Sample DetectionVisualizationBlottingQuantitative Electrophoresis17.8 - Enhancing ResolutionDisc ElectrophoresisIsoelectric Focusing2D Gel Electrophoresis TechniquesProfile - 2D Success17.9 - Capillary ElectrophoresisProfile - Capillary Electrophoresis and the Human Genome ProjectIntroduction to Capillary ElectrophoresisThe InstrumentSeparation EfficiencyElectroosmotic FlowSample Loading and ThroughputDynamic CoatingDetectionRecent Developments in CE Compare and Contrast: A look back at four different separation techniques17.10 - Useful DataTable 17.1 - Polyacrylamide Gel Separation RangesTable 17.2 - Stains for Gels17.11 - Further Reading17.12 - Additional ExercisesCHAPTER 18 - Potentiometry & Probes18.1 -Basic Principles: Probes and BiosensorsProfile- Handheld water quality probe18.2 - Potentiometric ProbesProfile - The Standard Hydrogen ElectrodeThe pH ProbeProfile - Nano-scale pH probe for in-vivo useThe Nitrate ProbeProfile - Construction of a Salicylate ISEThe Oxygen Probe18.3 - Non-potentiometric probesThe Dissolved OxygenThe Chloride ProbeThe Total Salinity Probe18.4 - Probes for Measurements in the Human BodyThe Glucose Probe - a BiosensorProfile- The Number of Adults Treated for Diabetes Doubled in a DecadeThe Alcohol Fuel Cell ProbeProfile - "Smart" Toilets18.5 - Further Reading18.6 - Additional ExercisesCHAPTER 19 - Analytical VoltammetryProfile - Behind Frankenstein19.1 - Basic PrinciplesProfile -Parsing Method Names19.2 - The Three-Cell Electrode Cell19.3 - ChronoamperometryThe ExperimentNoise in CA and Related MethodsCharging CurrentMass TransportControlling Mass TransportProfile - Chronoamperometric Nerve Gas SensorThe Cottrell EquationProfile - VX Probe19.4 - Linear Sweep and Cyclic VoltammetryProfile - The International Space Station Electronic TongueBackgroundThe ExperimentReversibilityQuantitative Analysis with CV - The Randles-Sevcik EquationQualitative Analysis with CVSolvents, Electrolytes and the Electrochemical Window19.5 - Square Wave Voltammetry19.6 - Working ElectrodesCommon Working ElectrodesUltramicroelectrodes and NanoelectrodesProfile - Cyclic Voltammetry in a Single Cell19.7 - Useful DataTemperature Dependence of Reference ElectrodesTemperature Dependence of Solvent Drying Techniques19.8 - Further Reading 19.9 -Additional ExercisesCHAPTER 20 - Material and Surface Analysis Techniques20.1- IntroductionProfile - Characterizing metal nanoparticles for water purification: electron microscopy in action 20.2- MicroscopyProfile - Microscopy and the Nobel Prize in PhysicsAtomic Force Microscopy (AFM) Profile - Controlling the shape of silver nanoparticles with pH- AFM in actionScanning Tunneling Microscopy (STM) Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) Compare and Contrast - Resolutions for different microscopy techniques20.3: Thermoanalytic TechniquesProfile-Thermogravimetric AnalysisDifferential Thermal Analysis (DTA) Thermogravimetric Analysis (TGA) Profile- TG/MSDifferential scanning calorimetry (DSC) Compare and Contrast: DTA, TGA, & DSCProfile - A Crime Scene Analysis20.4 - Mechanical Stress AnalysisDynamic Mechanical Analysis20.5- Further reading 20.6- Additional ExercisesCHAPTER 21 - Advanced Topics in NMR: Understanding the NMR Experiment21.1 - IntroductionProfile - Adriaan "Ad" Bax21.2 - Resonance in the Rotating Frame21.3 - The Pulse ExperimentRelaxation of the excited stateLongitudinal Relaxation (Spin-Lattice): T1Measuring T1: Inversion RecoveryTransverse Relaxation (Spin-Spin): T2Measuring T2: Spin-Echo21.4 - The Influence of Nuclear Neighbors:J-CouplingDipolar Coupling and The Nuclear Overhauser EffectProfile- Albert W. OverhauserProfile - Jean Jeener21.5 - Introduction to 2D NMRCOSY and TOSCYNOESYProfile - G. Marius CloreProfile - Kurt Wuthrich21.6 - Special Topics in NMRVariable Temperature NMRSolid State NMROther Spin-Active NucleiPhosphorus-31Nitrogen-15Platinum-195Fluorine-1921.7 - Useful Data21.8 - Further Reading21.9 - Additional ExercisesCHAPTER 22: Statistical Data Analysis22.1-Introduction22.2 -Types of ErrorGross ErrorSystematic ErrorRandom Error22.3 -Precision vs. Accuracy22.4 -Statistical ToolsPopulation vs. SampleMeanStandard Deviation and VarianceStandard Error and Error Bars. Normal DistributionsConfidence LimitsUsing Spreadsheets to Determine Confidence LimitsPropagation of ErrorData SetsIdentifying Outliers: The Q-TestIdentifying Outliers: The Grubb's TestAnalyzing Variance: The F-TestANOVA: A 2-Dimenstional F-Test22.5 -Linear Regression Analysis22.6 -LOD, LOQ, and LDR22.7 -Further Reading22.8 - Additional ExercisesAppendix: Table of Acronyms and AbreviationsIndex

I like this book's simplicity and the way it addresses its audience of predominantly undergraduate students. They key concepts were presented seamlessly with related topics for typical one-semester undergraduate instrumental analysis courses.