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Instrumental Analysis XE

Robert M. Granger, Hank M. Yochum, Jill N. Granger, and Karl D. Sienerth

October 2019

ISBN: 9780199942343

624 pages
Paperback
279x216mm

In Stock

Price: £54.99

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Description

Instrumental Analysis provides a rigorous, modern, and engaging coverage of chemical instrumentation, written with the undergraduate student in mind. It provides students with the requisite skills to identify the comparative advantages and disadvantages in choosing one analytical technique over another by combining direct comparisons of the techniques with a discussion of how these choices affect the interpretation of the data in its final form.

  • Provides comprehensive, modern, and engaging coverage of chemical instrumentation
  • Compare and Contrast Boxes: Compare and Contrast boxes directly compare different instrumental techniques to help students understand the trade-offs in choosing one technique over another
  • Profile Boxes: To capture the student's imagination, each chapter begins with a real world application, and additional profile boxes appear throughout the chapter
  • Activity Boxes: The text includes activity boxes that allow students to recreate a physical phenomenon or to build a working instrument component
  • Worked Examples: Each chapter contains several worked examples that walk the student through key calculations and exercises
  • Sample Problems: Placed in close proximity to each worked example feature, sample problems allow students to acquire their own expertise
  • Further Reading: Each chapter ends with a bibliography of influential texts and journal articles
  • Exercises: Exercises that reinforce key concepts appear throughout the chapters and at the end of the chapters

About the Author(s)

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

Robert M. Granger, II (Ph.D. Purdue University) is Chair and Professor of Chemistry at Sweet Briar College, where he teaches instrumental analysis and advanced inorganic courses. Jill N. Granger (Ph.D. Purdue University) is Professor of Chemistry at Sweet Briar College, where she teaches analytical chemistry, biochemistry, and chemistry for non-majors courses. Karl Sienerth (Ph.D. University of Tennessee, Knoxville) is Professor of Chemistry at Elon University, where he teaches quantitative analysis, instrumental analysis, and other analytical chemistry courses. Hank Yochum (Ph.D. Wake Forest University) is Associate Professor of Physics and Engineering and the Director of the Margaret Jones Wyllie '45 Engineering Program at Sweet Briar College where he teaches physical chemistry, general physics, optics, circuits, quantum mechanics, and more.

Table of Contents

    Preface
    Chapter 1. The Analyst's Toolbox
    Profile - A Scenario
    1.2 - Introduction
    1.2 - Ultraviolet - visible Spectroscopy
    1.3 - Infrared Spectroscopy
    Compare and Contrast - UV-vis vs. FTIR in Quantitative Analysis
    1.4 - Nuclear Magnetic Resonance Spectrometry
    1.5 - Mass Spectrometry
    Profile - Putting it All Together
    1.6 - Chromatography
    Profile - Establishing a Forensic Protocol
    1.7 - Additional Exercises
    Chapter 2. Quantum Mechanics and Spectroscopy
    Profile- The Brain Initiative and everyday spectroscopy
    2.1- Introduction
    2.2- The interaction between electromagnetic radiation and matter - absorption and emission of light
    Profile - Erwin Schrödinger
    2.3- Molecular vibrations lead to quantized energy levels
    Profile - London's Millennium Bridge
    Profile- Mass Dampers
    2.4- Molecular rotation leads to quantized energy levels
    2.5- Transitions between vibrational and rotational states -the role of thermal energy and nonradiative decay
    Prelude - The Boltzmann Distribution
    2.6- Transitions between electronic, vibrational, and rotational states - putting it all together
    The Jablonski diagram
    Fluorescence and Phosphorescence
    2.7 Energy levels of a proton in a magnetic field - Nuclear Magnetic Resonance (NMR) Spectroscopy
    2.8- Additional Exercises
    Chapter 3. An Introduction to Optics
    Profile: The diffraction grating is a key component for many optical instruments
    3.1 - An Introduction to the Properties of Light
    Wavelength, Energy, and Frequency
    Coherence
    Polarization
    Interference
    Diffraction
    Scattering
    Profile- The photoelectric effect shows the particle nature of light
    3.2- Controlling optical beams
    Mirrors and Reflection
    Lenses and Refraction
    Collecting and Collimating Light
    Focusing a Collimated Laser Beam
    Polarizers
    3.3- Wavelength Selection
    Introduction to Prism and Grating Monochromators
    The Diffraction Grating
    Putting it all together- Details on the Grating Monochromator
    Profile- Optics that operate by diffraction- the Fresnel Zone Plate
    The Michelson Interferometer
    Optical Filters & Power Reduction
    3.4 - Common Optical Materials
    3.5- Beyond Linear Optics
    Profile- Innovation and discovery in optics - metamaterials hold promise for the perfect lens, invisibility cloaks, and more
    3.6 - Additional Exercises
    Chapter 4. An Introduction to Instrumental Electronics
    4.1 - Introduction
    Circuit Symbols
    4.2 - DC Circuits
    Current, Voltage, and Multimeter Basics
    Series Circuit Elements and the Voltage Divider
    Parallel Circuit Elements and the Current Divider
    The Multimeter
    Voltage and Current Loading Error
    Profile - Electronics for a Very Simple Light Sensing Instrument: Voltage Divider Photoresistor circuit
    4.3- Capacitors and RC Circuits
    4.4- AC Circuits
    Ohm's law for AC circuits
    Low-pass, High-pass, Band-pass, and Band Stop Filters
    Activity- RC Filter Spreadsheet Tool
    4.5 - Operational Amplifiers
    Inverting and Non-inverting op amps
    Summing op amp
    Current to Voltage Amplifier
    The Voltage Follower
    Op Amp Comparator
    Cascading op amps
    A Cascaded Op Amp Example- Instrumentation Op Amp
    Profile- Electronics for an Automatic Titrator: Cascaded Op Amps and the Differentiating Op Amp
    4.6 - Quick Survey of Components
    Potentiometers
    Diode
    Transistors
    Profile- Electronics for a Simple Absorption Spectrophotometer: Op Amp Circuit as Current to Voltage Amplifier
    Profile- What if you need a constant voltage under varying loads? A basic schematic of a potentiostat
    4.7 - Analog and Digital Signals
    4.8 - Additional Exercises
    Chapter 5. Signals and Noise: An Introduction to Signal Processing
    Profile- Spectroscopy of single molecules?
    5.1 - Introduction to Signals
    5.2 - Sources and Characteristics of Noise
    5.3 - Signal to Noise Ratio and Ensemble Averaging
    5.4- Processing Signals with Hardware and Software
    Analog Filters
    Boxcar averaging with hardware
    Modulating Signals and the Lock-In Amplifier
    Digital Filters
    Rolling average, Boxcar average, Savitzky-Golay Filter, and Fourier Filtering
    5.5 - Sampling Rates, the Nyquist Frequency, and Aliasing
    5.6- Analog to Digital Conversion
    5.7 - Additional Exercises
    Chapter 6. Molecular Ultraviolet and Visible Spectroscopy
    Profile - James Clerk Maxwell
    6.1 - Introduction
    6.2 - Electronic Excitation and Molecular Structure
    Structure and "Color"
    Heteroatoms
    DPK - A Case Study
    Solvent Polarity
    Transition Metal Coordination Compounds
    Vibronic Transitions
    Sidebar - The Spectroscopic Series
    6.3 - Quantitative Measurements
    Selection Rules
    Beer's Law
    Sidebar - Derivation of Beer's Law
    Deviations from Beer's Law
    Bandwidth Resolution
    Activity - Explore the effects on the relationship of A vs. c
    6.4 - Instrumentation Designs
    Fixed Wavelength Spectrometers
    Profile - HACH DR3900
    Scanning Spectrometers
    Compare and Constrast - Single & Dual Beam Spectrometers
    Array Spectrophotometers
    6.5 - Monochromators
    6.6 - Sources
    Deuterium Arc/Tungsten Halogen Bulb
    Xenon Arc Lamps
    Light Emitting Diodes
    Profile - The Jaz® by Ocean Optics
    6.7 - Detectors
    The PMT
    Photovoltaic Cells
    Charge Coupled Device
    6.8 - Noise
    Stray Light
    Detector Noise
    Profile - Walter Hermann Schottky
    Source Noise
    6.9 - Kinetic UV-vis Techniques
    Stop Flow UV-vis
    Flash Photolysis
    Profile - Building a functional monochromator
    6.10 - Useful Data
    6.11 - Additional Exercises
    Chapter 7. Atomic Absorption Spectroscopy
    7.1- Introduction
    Profile - The Birth of Atomic Absorption Spectroscopy (AAS)
    7.2 - Molecular vs. Atomic Absorption
    Analytical Specificity
    7.3 - Spectral Bandwidth
    Lifetime Broadening
    Profile - Review of Term Symbols
    Magnetic Field Broadening
    Profile - Lightning over Salty Waters
    Pressure Broadening
    Note - IUPAC nomenclature for pressure broadening.
    Doppler Broadening
    7.4 -AAS Sources
    The Hollow-Cathode Lamp
    Profile - Nutritional Contents of Breast Milk
    Electrodeless Discharge Lamps
    Activity - Soil Analysis
    7.5 - Sample Introduction
    Flame - AAS
    The Flame
    The Flame Height
    Electrothermal-AAS/GFAAS
    Flame vs Electrothermal AAS
    Profile- AAS Analysis of Oil
    Hydride - AAS
    Cold Vapor-AAS
    Compare and Contrast - Detection Limit Ranges
    7.6 - Measuring Atomic Absorption
    Background Correction
    Zeeman Background Correction
    Smith-Hieftje background correction
    Spectral Interference
    Profile-Demystifying the Zeeman Effect
    7.7 - Sample Preparation
    Acid Digestion
    7.8 - Performing an AAS analysis
    7.9 - Additional Exercises
    Chapter 8. Luminescence Spectroscopy
    8.1 - Introduction
    8.2 - Theory
    Principles of Fluorescence and Phosphorescence
    Profile - Is your $100 bill real? Find out with time-resolved fluorescence
    Relating fluorescence and molecular structure
    Profile - Fluorescence quenching helps with aerodynamics
    8.3 -The Fluorescence Spectrometer
    Excitation sources
    Wavelength discrimination and instrument resolution
    Detectors
    Putting it all together- Walking through the luminescence system
    Excitation spectra
    Sample introduction
    Profile- Fluorescence pushes the limits of detection- single molecule detection and femtomolar concentrations
    8.4- Challenges with Fluorescence Spectroscopy
    Detector response correction
    Source intensity correction
    Stray light contamination
    Challenges with high absorbance
    Photobleaching
    8.5 -Additional Fluorescence based techniques
    Chemiluminescence
    Fluorescence polarization
    Resonance energy transfer spectroscopy
    Multiphoton excitation
    8.6 - Additional Exercises
    Profile - Using fluorescence to determine concentrations of DNA and RNA
    Chapter 9. Atomic Emission Spectroscopy
    9.1 - Introduction
    Profile - Get The Lead Out
    9.2 - The Atomizer and the Excitation Source
    Profile - Columbia
    Inductively Coupled Plasma Torch
    Direct Current Plasma Source
    Profile - The Plasma Torch
    Microwave Induced Plasma Source
    Profile - Atmospheric MP-AES
    Profile - LIBS in Space
    Laser Ablation
    Profile- Visualizing a Plasma
    9.3 - Sample Introduction
    Applications
    Sources AAS vs. AES
    Sample preparation and interferences
    Zeeman Background Correction
    9.4 - Measuring Atomic Emission
    Compare and Contrast FAAS, GFAAS & ICP-AES
    9.5- Additional Exercises
    Chapter 10. Infrared Spectroscopy
    10.1 -Chemical Structure and Molecular Vibrations
    Profile - The Future of FTIR
    Wavenumbers
    Group Frequencies
    Normal Modes
    Vibrational Categories
    Profile - Olive Oil
    The Selection Rules and Molecular Symmetry
    Vibronic Coupling
    10.2 - Time Domain vs. Frequency Domain Spectroscopy: The Fourier Transformation
    Activity: Creating a Beat Pattern
    Activity: Performing a Fourier Transform
    10.3 -FTIR & Wavelength Discrimination
    The Michelson Interferometer
    Resolution
    Activity: Exploring Resolution
    10.4 -Sources
    The Nernst Glower
    The Globar
    Coiled Wire Sources
    Solid State Sources
    10.5 -Detectors
    Thermal Detectors
    Pyroelectric Detectors
    Profile- PZT Ceramics
    Photoconductive Detectors
    Profile- MCT Detectors
    Quantum Well Detectors
    10.6 -Spectral Output
    Transmittance vs. Absorbance
    Quantitative Measurements and Deviations from Beer's Law
    10.7- Developments; Two Dimensional Infrared Spectroscopy
    10.8 - Sample Introduction
    Optical Materials
    Gasses
    Solution IR Spectroscopy
    Neat Liquids
    Solids
    ATR
    Compare and Contrast: UV-vis versus FTIR in Quantitative & Qualitative Analysis
    10.9 - Useful Data
    10.10- Additional Exercises
    Chapter 11. Raman Spectroscopy
    Profile - Raman Applications in Art and Medicine
    11.1 -Introduction
    Rayleigh Scattering
    11.2 - Theory of Raman Scattering
    Selection Rules
    Case Study - Vibrations in the linear molecule CO2
    Case Study- Raman spectroscopy of a tetrahedral molecule; CCl4
    11.3 -The Raman Spectrometer
    Instrument Basics
    Radiant Source
    Wavelength Discrimination and Raman
    Spectrometer Resolution
    Filters
    Detectors
    Compare and Contrast - A side-by-side evaluation of FTIR and Raman spectroscopy.
    Handheld Raman Analyzers
    Profile - Drug detection using commercial handheld Raman spectrometers
    Fiber optic probes
    11.4- Additional Raman based techniques
    Raman Imaging
    Polarized Raman Spectroscopy
    Fourier Transform Raman Spectroscopy (FT-Raman)
    Surface enhanced Raman Spectroscopy (SERS)
    Profile - Using Raman spectroscopy to identify compounds from a distance
    11.5 - Additional Exercises
    Chapter 12. Mass Spectrometry
    12.1 - Basic Principles & Comparisons to an Optical Spectrophotometer
    Profile - Puffer MS
    12.2 - Ion sources
    Electron Ionization
    Profile - J. J. Thomson
    Chemical Ionization
    Electrospray Ionization
    Profile - John Fenn
    Matrix Assisted Laser Desorption Ionization
    Secondary Ion
    Thermal Ionization
    Inductively Coupled Plasma
    Compare & Contrast - Elemental Methods
    Profile - TOF-MS in Space
    12.3 - Mass Analyzers
    Sector & Double-focusing
    Profile - Eugen Goldstein Quadrupole
    Profile - R. Graham Cooks
    Time-of-flight
    FT Ion Cyclotron Resonance
    12.4 - Detectors
    Activity - Selected Ion Game
    12.5 - Additional Techniques
    Tandem Techniques
    Isotope Ratio Mass Spectrometry
    Accelerator Mass Spectrometry
    Profile - 10Be as a Geological Clock
    Profile - Human Scent Fingerprinting
    12.6 - Additional Exercises
    Advanced Exercises
    Chapter 13. An Introduction to Nuclear Magnetic Resonance Spectroscopy
    13.1 - Introduction
    Profile - NMR versus HIV
    Spectral Analysis - A Quick Review
    13.2 - NMR Spectroscopy is all about the Nucleus
    Nuclear Quantum Numbers
    A Nucleus in a Magnetic Field
    Tesla vs. MHz
    13.3 - The NMR Signal
    Compare and Contrast - Population distribution for common spectroscopic methods
    Profile - Felix Bloch
    13.4 - The RF Pulse: Inducing nuclear magnetic resonance
    FT-NMR: Time Domain vs. Frequency Domain Spectroscopy & The Fourier Transformation
    Free Induction Decay (FID): The FT-NMR "Beat Pattern"
    13.5 - Chemical Shift and Resolution
    Profile - Richard R. Ernst
    The Chemical Shift (ppm)
    Chemical Shift Reference
    Resolution
    13.6 - The Instrument
    Shimming
    Loading
    13.7 - Signal Processing
    Increasing the signal to noise ratio
    Profile - Angela Gronenborn
    13.8 - Magnetic Resonance Imaging
    Profile - MRI and Brain Concussion
    Texts
    On Line Resources
    Some interesting laboratory experiments
    13.9 - Additional Exercises
    Chapter 14. Liquid Chromatography
    14.1 - Introduction
    Profile- Mikhail S. Tswett
    14.2 - Theory
    Distribution Equilibrium
    Profile - Other Applications of Partition Coefficients
    Principles of Chromatography
    Activity: TLC at home
    The Retention Factor
    Resolution and Theoretical Plates
    Band Broadening
    14.3 - Basic Method Development
    Thermodynamics and Kinetics Factors
    Isocratic vs. Gradient
    Profile: The Role of Temperature
    Qualitative vs. Quantitative
    Profile: Analysis of Wine - Qualitative and Quantitative
    14.4 - Stationary Phase Materials and Modes of Separation
    Profile: LC-MS in Athletic Doping
    Normal Phase
    Reversed Phase
    Ion Exchange
    Hydrophilic Interaction Chromatography (HIC)
    Affinity
    Chiral Chromatography
    Profile - The Chiral Medicine Cabinet
    Size Exclusion
    14.5 - Instrumentation
    Overview
    HPLC Components
    Profile -Ultrahigh Pressure LC
    Mobile Phase
    Columns
    Injectors
    Pumps
    Detectors
    Profile- Major Players, the Chromatography Industry
    14.7 - Additional Exercises
    Chapter 15. Gas Chromatography
    Profile - Odorants, Pheromones, and Chemosignals
    15.1 - Introduction
    Profile - Gas Chromatography on Mars
    15.2 - Basic GC Instrument Design
    15.3 - Method Development: a case study
    A Case Study - Peanut Butter
    Profile - The NIST 14 Gas Chromatography (GC) Library with Search Software
    15.4 - Modes of Separation
    Isothermal vs. Temperature gradients
    The Column
    15.5 - Carrier Gas and Injector
    Carrier Gases
    15.6 - Detectors
    Ionizing Detectors
    Optical Detectors
    Thermal Conductivity Detectors
    Electrochemical Detectors
    Tandem Instrument Detection
    Quantitative and Qualitative Considerations
    15.7 - New Developments and Directions in GC
    Multidimensional GC Techniques
    Profile - Breath and Air Quality
    Miniaturization, Portability, Speed, and Throughput
    15.8 - Extended Theory
    Evaluation of the GC Separation
    The Relationship between VN, k, and Selectivity
    The General Elution Problem
    15.9 - Useful Information
    Table 16.3 - GC column Manufacturers
    15.10 - Additional Exercises
    Chapter 16. Electrophoresis
    16.1 - Introduction
    Profile - The Father of Electrophoresis
    16.2 - Fundamental Principles
    16.3 - The Basic Apparatus
    Profile - DNA Markers
    16.4 - Paper Electrophoresis
    Activity -Demystifying Electrophoresis: Build Your Own Electrophoresis Apparatus
    16.5 - Gel Electrophoresis
    Polyacrylamide Gel Electrophoresis (PAGE)
    SDS PAGE
    Agarose Gel Electrophoresis
    16.6 - Ending the Analysis: The Time Factor
    16.7 - Gel Sample Detection
    Visualization
    Blotting
    Quantitative Electrophoresis
    16.8 - Enhancing Resolution
    Disc Electrophoresis
    Isoelectric Focusing
    2D Gel Electrophoresis Techniques
    Profile - 2D Success
    16.9 - Capillary Electrophoresis
    Profile - Capillary Electrophoresis and the Human Genome Project
    Introduction to Capillary Electrophoresis
    The Instrument
    Separation Efficiency
    Electroosmotic Flow
    Sample Loading and Throughput
    Dynamic Coating
    Detection
    Recent Developments in CE
    Compare and Contrast: A look back at four different separation techniques
    16.10 - Useful Data
    Table 16.1 - Polyacrylamide Gel Separation Ranges
    Table 16.2 - Stains for Gels
    16.11 - Additional Exercises
    Chapter 17. Potentiometry & Probes
    17.1 -Basic Principles: Probes and Biosensors
    Profile- Handheld water quality probe
    17.2 - Potentiometric Probes
    Profile - The Standard Hydrogen Electrode
    The pH Probe
    Profile - Nano-scale pH probe for in-vivo use
    The Nitrate Probe
    Profile - Construction of a Salicylate ISE
    The Oxygen Probe
    17.3 - Non-potentiometric probes
    The Dissolved Oxygen
    The Chloride Probe
    The Total Salinity Probe
    17.4 - Probes for Measurements in the Human Body
    The Glucose Probe - a Biosensor
    Profile- The Number of Adults Treated for Diabetes Doubled in a Decade
    The Alcohol Fuel Cell Probe
    Profile - "Smart" Toilets
    17.5 - Additional Exercises
    Chapter 18: Statistical Data Analysis
    18.1-Introduction
    18.2 -Types of Error
    Gross Error
    Systematic Error
    Random Error
    18.3 -Precision vs. Accuracy
    18.4 -Statistical Tools
    Population vs. Sample
    Mean
    Standard Deviation and Variance
    Standard Error and Error Bars.
    Normal Distributions
    Confidence Limits
    Using Spreadsheets to Determine Confidence Limits
    Propagation of Error
    Data Sets
    Identifying Outliers: The Q-Test
    Identifying Outliers: The Grubb's Test
    Analyzing Variance: The F-Test
    ANOVA: A 2-Dimenstional F-Test
    18.5 -Linear Regression Analysis
    18.6 -LOD, LOQ, and LDR
    18.7 - Additional Exercises
    Index

Reviews

"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." - Dan Sykes, Pennsylvania State University

"Instrumental Analysis is a much-needed introductory undergraudate textbook. It provides sufficient introductrory information for undergraduates along with crucial emphasis on microscale, nano, portable, and other new instrumetation. This text covers everything, the organization is clear, and the writing is easy to understand." - Tami Lasseter Clare, Portland State University