Fundamentals of Analytical Chemistry

Höfundur: Douglas Skoog (Útgáfa: 10)
Fundamentals of Analytical Chemistry

Kaup valmöguleikar

Introduce the principles and practices behind analytical chemistry while emphasizing its applied nature with Skoog/West/Holler/Crouch's FUNDAMENTALS OF ANALYTICAL CHEMISTRY, 10th Edition. This award-winning author team presents analytical chemistry using a reader-friendly yet systematic and rigorous approach with updates that reflect the latest developments. Each chapter begins with a compelling story and stunning visuals that demonstrate how analytical chemistry impacts industry, medicine and the sciences today.

Nánar um bókina

Útgefandi
Cengage Learning US
ISBN
9798214344171
Print ISBN
9780357450390
Format
ePub
Útgáfa
10
Höfundar
Douglas Skoog
Tungumál
English
Útgefið
2021-08-04
Prent takmörkun á líftíma
100

Kaflar

  • Cover Page
  • Title Page
  • Copyright Page
  • Endpapers
  • Preface
  • Part I. Tools of Analytical Chemistry
  • Chapter 1. The Nature of Analytical Chemistry
  • 1A. The Role of Analytical Chemistry
  • 1B. Quantitative Analytical Methods
  • 1C. A Typical Quantitative Analysis
  • 1C-1. Choosing a Method
  • 1C-2. Acquiring the Sample
  • 1C-3. Processing the Sample
  • 1C-4. Eliminating Interferences
  • 1C-5. Calibrating and Measuring Concentration
  • 1C-6. Calculating Results
  • 1C-7. Evaluating Results by Estimating Reliability
  • 1D. An Integral Role for Chemical Analysis: Feedback Control Systems
  • Chapter 1. Summary
  • Key Terms
  • Important Equations
  • Chapter 2. Calculations Used in Analytical Chemistry
  • 2A. Some Important Units of Measurement
  • 2A-1. SI Units
  • 2A-2. The Distinction between Mass and Weight
  • 2A-3. The Mole
  • 2A-4. The Millimole
  • 2A-5. Calculating the Amount of a Substance in Moles or Millimoles
  • 2B. Solutions and Their Concentrations
  • 2B-1. Concentration of Solutions
  • 2B-2. Density and Specific Gravity of Solutions
  • 2C. Chemical Stoichiometry
  • 2C-1. Empirical Formulas and Molecular Formulas
  • 2C-2. Stoichiometric Calculations
  • 2D. Calculations Using Microsoft® Excel
  • Chapter 2. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 3. Precision and Accuracy of Chemical Analyses
  • 3A. Some Important Terms
  • 3A-1. The Mean and the Median
  • 3A-2. Precision
  • 3A-3. Accuracy
  • 3A-4. Types of Errors in Experimental Data
  • 3B. Systematic Errors
  • 3B-1. Sources of Systematic Errors
  • 3B-2. The Effect of Systematic Errors on Analytical Results
  • 3B-3. Detection of Systematic Instrument and Personal Errors
  • 3B-4. Detection of Systematic Method Errors
  • Chapter 3. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 4. Random Errors in Chemical Analysis
  • 4A. The Nature of Random Errors
  • 4A-1. Random Error Sources
  • 4A-2. Distribution of Experimental Results
  • 4B. Statistical Treatment of Random Errors
  • 4B-1. Samples and Populations
  • 4B-2. Properties of Gaussian Curves
  • 4B-3. The Sample Standard Deviation: A Measure of Precision
  • 4B-4. Reliability of s as a Measure of Precision
  • 4B-5. Variance and Other Measures of Precision
  • 4C. Standard Deviation of Calculated Results
  • 4C-1. Standard Deviation of a Sum or Difference
  • 4C-2. Standard Deviation of a Product or Quotient
  • 4C-3. Standard Deviations in Exponential Calculations
  • 4C-4. Standard Deviations of Logarithms and Antilogarithms
  • 4D. Reporting Computed Data
  • 4D-1. Significant Figures
  • 4D-2. Significant Figures in Numerical Computations
  • 4D-3. Rounding Data
  • 4D-4. Expressing Results of Chemical Calculations
  • Chapter 4. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 5. Statistical Data Treatment and Evaluation
  • 5A. Confidence Intervals
  • 5A-1. Finding the Confidence Interval When σ Is Known or s Is a Good Estimate of σ
  • 5A-2. Finding the Confidence Interval When σ Is Unknown
  • 5B. Statistical Aids to Hypothesis Testing
  • 5B-1. Comparing an Experimental Mean with a Known Value
  • 5B-2. Comparison of Two Experimental Means
  • 5B-3. Errors in Hypothesis Testing
  • 5B-4. Comparison of Variances
  • 5C. Analysis of Variance
  • 5C-1. ANOVA Concepts
  • 5C-2. Single-Factor ANOVA
  • 5C-3. Determining Which Results Differ
  • 5D. Detection of Gross Errors
  • 5D-1. The Q Test
  • 5D-2. Other Statistical Tests
  • 5D-3. Recommendations for Treating Outliers
  • Chapter 5. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 6. Sampling, Standardization, and Calibration
  • 6A. Analytical Samples and Methods
  • 6A-1. Types of Samples and Methods
  • 6A-2. Real Samples
  • 6B. Sampling
  • 6B-1. Obtaining a Representative Sample
  • 6B-2. Sampling Uncertainties
  • 6B-3. The Gross Sample
  • 6B-4. Preparing a Laboratory Sample
  • 6B-5. Number of Laboratory Samples
  • 6C. Automated Sample Handling
  • Discrete Methods
  • 6D. Standardization and Calibration
  • 6D-1. Comparison with Standards
  • 6D-2. External Standard Calibration
  • 6D-3. Minimizing Errors in Analytical Procedures
  • 6E. Figures of Merit for Analytical Methods
  • 6E-1. Sensitivity and Detection Limit
  • 6E-2. Linear Dynamic Range
  • 6E-3. Quality Assurance of Analytical Results
  • Chapter 6. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Part II. Chemical Equilibria
  • Chapter 7. Aqueous Solutions and Chemical Equilibria
  • 7A. The Chemical Composition of Aqueous Solutions
  • 7A-1. Classifying Solutions of Electrolytes
  • 7A-2. Acids and Bases
  • 7A-3. Amphiprotic Species
  • 7A-4. Autoprotolysis
  • 7A-5. Strengths of Acids and Bases
  • 7B. Chemical Equilibrium
  • 7B-1. The Equilibrium State
  • 7B-2. Equilibrium-Constant Expressions
  • 7B-3. Types of Equilibrium Constants in Analytical Chemistry
  • 7B-4. Applying the Ion-Product Constant for Water
  • 7B-5. Using Solubility-Product Constants
  • 7B-6. Using Acid-Base Dissociation Constants
  • 7C. Buffer Solutions
  • 7C-1. Calculating the pH of Buffer Solutions
  • 7C-2. Properties of Buffer Solutions
  • Chapter 7. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 8. Effect of Electrolytes on Chemical Equilibria
  • 8A. The Effect of Electrolytes on Chemical Equilibria
  • 8A-1. The Effect of Ionic Charges on Equilibria
  • 8A-2. The Effect of Ionic Strength
  • 8A-3. The Salt Effect
  • 8B. Activity Coefficients
  • 8B-1. Properties of Activity Coefficients
  • 8B-2. The Debye-Hückel Equation
  • 8B-3. Equilibrium Calculations Using Activity Coefficients
  • 8B-4. Omitting Activity Coefficients in Equilibrium Calculations
  • Chapter 8. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 9. Solving Equilibrium Problems for Complex Systems
  • 9A. Solving Multiple-Equilibrium Problems Using a Systematic Method
  • 9A-1. Mass-Balance Equations
  • 9A-2. Charge-Balance Equation
  • 9A-3. Steps for Solving Problems with Several Equilibria
  • 9A-4. Using Approximations to Solve Equilibrium Calculations
  • 9A-5. Use of Computer Programs to Solve Multiple-Equilibrium Problems
  • 9B. Calculating Solubilities by the Systematic Method
  • 9B-1. The Solubility of Metal Hydroxides
  • 9B-2. The Effect of pH on Solubility
  • 9B-3. The Effect of Undissociated Solutes on Precipitation Calculations
  • 9B-4. The Solubility of Precipitates in the Presence of Complexing Agents
  • 9C. Separation of Ions by Control of the Concentration of the Precipitating Agent
  • 9C-1. Calculation of the Feasibility of Separations
  • 9C-2. Sulfide Separations
  • Chapter 9. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Part III. Classical Methods of Analysis
  • Chapter 10. Gravimetric Methods of Analysis
  • 10A. Precipitation Gravimetry
  • 10A-1. Properties of Precipitates and Precipitating Reagents
  • 10A-2. Desirable Properties of Precipitates
  • 10A-3. Colloidal Precipitates
  • 10A-4. Crystalline Precipitates
  • 10A-5. Coprecipitation
  • 10A-6. Precipitation from Homogeneous Solution
  • 10A-7. Drying and Ignition of Precipitates
  • 10B. Calculation of Results from Gravimetric Data
  • 10C. Applications of Gravimetric Methods
  • 10C-1. Inorganic Precipitating Agents
  • 10C-2. Reducing Agents
  • 10C-3. Organic Precipitating Agents
  • 10C-4. Organic Functional Group Analysis
  • 10C-5. Volatilization Gravimetry
  • Chapter 10. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 11. Titrations in Analytical Chemistry
  • 11A. A Some Terms Used in Volumetric Titrations
  • 11A-1. Equivalence Points and End Points
  • 11A-2. Primary Standards
  • 11B. Standard Solutions
  • 11C. Volumetric Calculations
  • 11C-1. Some Useful Relationships
  • 11C-2. Calculating the Molar Concentration of Standard Solutions
  • 11C-3. Working with Titration Data
  • 11D. Gravimetric Titrations
  • 11D-1. Calculations Associated with Mass Titrations
  • 11D-2. Advantages of Gravimetric Titrations
  • 11E. Titration Curves
  • 11E-1. Types of Titration Curves
  • 11E-2. Concentration Changes During Titrations
  • Chapter 11. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 12. Principles of Neutralization Titrations
  • 12A. Solutions and Indicators for Acid-Base Titrations
  • 12A-1. Standard Solutions
  • 12A-2. Acid-Base Indicators
  • 12B. Titration of Strong Acids and Bases
  • 12B-1. Titrating a Strong Acid with a Strong Base
  • 12B-2. Titrating a Strong Base with a Strong Acid
  • 12C. Titration Curves for Weak Acids
  • 12C-1. The Effect of Concentration
  • 12C-2. The Effect of Reaction Completeness
  • 12C-3. Choosing an Indicator: The Feasibility of Titration
  • 12D. Titration Curves for Weak Bases
  • 12E. The Composition of Solutions During Acid-Base Titrations
  • Chapter 12. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 13. Complex Acid-Base Systems
  • 13A. Mixtures of Strong and Weak Acids or Strong and Weak Bases
  • 13B. Polyfunctional Acids and Bases
  • 13B-1. The Phosphoric Acid System
  • 13B-2. The Carbon Dioxide/Carbonic Acid System
  • 13C. Buffer Solutions Involving Polyprotic Acids
  • 13D. Calculation of the pH of Solutions of NaHA
  • 13E. Titration Curves for Polyfunctional Acids
  • 13F. Titration Curves for Polyfunctional Bases
  • 13G. Titration Curves for Amphiprotic Species
  • 13H. Composition of Polyprotic Acid Solutions as a Function of pH
  • Chapter 13. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 14. Applications of Neutralization Titrations
  • 14A. Reagents for Neutralization Titrations
  • 14A-1. Preparation of Standard Acid Solutions
  • 14A-2. The Standardization of Acids
  • 14A-3. Preparation of Standard Solutions of Base
  • 14A-4. The Standardization of Bases
  • 14B. Typical Applications of Neutralization Titrations
  • 14B-1. Elemental Analysis
  • 14B-2. The Determination of Inorganic Substances
  • 14B-3. The Determination of Organic Functional Groups
  • 14B-4. The Determination of Salts
  • Chapter 14. Summary
  • Key Terms
  • Questions and Problems
  • Chapter 15. Complexation and Precipitation Reactions and Titrations
  • 15A. The Formation of Complexes
  • 15A-1. Complexation Equilibria
  • 15A-2. The Formation of Insoluble Species
  • 15A-3. Ligands That Can Protonate
  • 15B. Titrations with Inorganic Complexing Agents
  • 15B-1. Complexation Titrations
  • 15B-2. Precipitation Titrations
  • 15C. Organic Complexing Agents
  • 15D. Aminocarboxylic Acid Titrations
  • 15D-1. Ethylenediaminetetraacetic Acid (EDTA)
  • 15D-2. Complexes of EDTA and Metal Ions
  • 15D-3. Equilibrium Calculations Involving EDTA
  • 15D-4. EDTA Titration Curves
  • 15D-5. The Effect of Other Complexing Agentson EDTA Titration Curves
  • 15D-6. Indicators for EDTA Titrations
  • 15D-7. Titration Methods Involving EDTA
  • 15D-8. The Scope of EDTA Titrations
  • 15D-9. Determination of Water Hardness
  • Chapter 15. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Part IV. Electrochemical Methods
  • Chapter 16. Introduction to Electrochemistry
  • 16A. Characterizing Oxidation/Reduction Reactions
  • 16A-1. Comparing Redox Reactions to Acid-Base Reactions
  • 16A-2. Oxidation/Reduction Reactions in Electrochemical Cells
  • 16B. Electrochemical Cells
  • 16B-1. Cathodes and Anodes
  • 16B-2. Types of Electrochemical Cells
  • 16B-3. Representing Cells Schematically
  • 16B-4. Currents in Electrochemical Cells
  • 16C. Electrode Potentials
  • 16C-1. Sign Convention for Cell Potentials
  • 16C-2. The Standard Hydrogen Reference Electrode
  • 16C-3. Electrode Potential and Standard Electrode Potential
  • 16C-4. Additional Implications of the IUPAC Sign Convention
  • 16C-5. Effect of Concentration on Electrode Potentials: The Nernst Equation
  • 16C-6. The Standard Electrode Potential, E 0
  • 16C-7. Limitations to the Use of Standard Electrode Potentials
  • Chapter 16. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 17. Applications of Standard Electrode Potentials
  • 17A. Calculating Potentials of Electrochemical Cells
  • 17B. Determining Standard Potentials Experimentally
  • 17C. Calculating Redox Equilibrium Constants
  • 17D. Constructing Redox Titration Curves
  • 17D-1. Electrode Potentials During Redox Titrations
  • 17D-2. The Titration Curve
  • 17D-3. Effect of Variables on Redox Titration Curves
  • 17E. Oxidation/Reduction Indicators
  • 17E-1. General Redox Indicators
  • 17E-2. Specific Indicators
  • 17F. Potentiometric End Points
  • Chapter 17. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 18. Applications of Oxidation/Reduction Titrations
  • 18A. Auxiliary Oxidizing and Reducing Reagents
  • 18A-1. Auxiliary Reducing Reagents
  • 18A-2. Auxiliary Oxidizing Reagents
  • 18B. Applying Standard Reducing Agents
  • 18B-1. Iron(II) Solutions
  • 18B-2. Sodium Thiosulfate
  • 18C. Applying Standard Oxidizing Agents
  • 18C-1. The Strong Oxidants: Potassium Permanganate and Cerium(IV)
  • 18C-2. Potassium Dichromate
  • 18C-3. Iodine
  • 18C-4. Potassium Bromate as a Source of Bromine
  • 18C-5. Determining Water with the Karl Fischer Reagent
  • Chapter 18. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 19. Potentiometry
  • 19A. General Principles
  • 19B. Reference Electrodes
  • 19B-1. Calomel Reference Electrodes
  • 19B-2. Silver/Silver Chloride Reference Electrodes
  • 19C. Liquid Junction Potentials
  • 19D. Indicator Electrodes
  • 19D-1. Metallic Indicator Electrodes
  • 19D-2. Membrane Indicator Electrodes
  • 19D-3. The Glass Electrode for Measuring pH
  • 19D-4. Glass Electrodes for Other Cations
  • 19D-5. Liquid-Membrane Electrodes
  • 19D-6. Crystalline-Membrane Electrodes
  • 19D-7. Ion-Sensitive Field Effect Transistors (ISFETS)
  • 19D-8. Gas-Sensing Probes
  • 19E. Instruments for Measuring Cell Potential
  • 19F. Direct Potentiometry
  • 19F-1. Equations Governing Direct Potentiometry
  • 19F-2. The Electrode-Calibration Method
  • 19F-3. The Standard Addition Method
  • 19F-4. Potentiometric pH Measurement with the Glass Electrode
  • 19G. Potentiometric Titrations
  • 19G-1. Detecting the End Point
  • 19G-2. Neutralization Titrations
  • 19G-3. Oxidation/Reduction Titrations
  • 19H. Potentiometric Determination of Equilibrium Constants
  • Chapter 19. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 20. Bulk Electrolysis: Electrogravimetry and Coulometry
  • 20A. The Effect of Current on Cell Potential
  • 20A-1. Ohmic Potential: IR Drop
  • 20A-2. Polarization Effects
  • 20B. The Selectivity of Electrolytic Methods
  • 20C. Electrogravimetric Methods
  • 20C-1. Electrogravimetry without Potential Control
  • 20C-2. Controlled-Potential Electrogravimetry
  • 20D. Coulometric Methods
  • 20D-1. Determining the Electrical Charge
  • 20D-2. Characterizing Coulometric Methods
  • 20D-3. Current Efficiency Requirements
  • 20D-4. Controlled-Potential Coulometry
  • 20D-5. Coulometric Titration
  • Chapter 20. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 21. Voltammetry
  • 21A. Excitation Signals in Voltammetry
  • 21B. Voltammetric Instrumentation
  • 21B-1. Working Electrodes
  • 21B-2. Modified Electrodes
  • 21B-3. Voltammograms
  • 21C. Hydrodynamic Voltammetry
  • 21C-1. Concentration Profiles at Electrode Surfaces
  • 21C-2. Voltammetric Currents
  • 21C-3. Oxygen Waves
  • 21C-4. Applications of Hydrodynamic Voltammetry
  • 21D. Polarography
  • Polarographic Currents
  • 21E. Cyclic Voltammetry
  • Fundamental Studies
  • 21F. Pulse Voltammetry
  • 21F-1. Differential-Pulse Voltammetry
  • 21F-2. Square-Wave Voltammetry
  • 21G. Applications of Voltammetry
  • 21G-1. Inorganic Applications
  • 21G-2. Organic Voltammetric Analysis
  • 21H. Stripping Methods
  • 21H-1. Electrodeposition Step
  • 21H-2. Voltammetric Completion of the Analysis
  • 21I. Voltammetry with Microelectrodes
  • Chapter 21. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Part V. Spectrochemical Analysis
  • Chapter 22. Introduction to Spectrochemical Methods
  • 22A. Properties of Electromagnetic Radiation
  • 22A-1. Wave Properties
  • 22A-2. The Particle Nature of Light: Photons
  • 22B. Interaction of Radiation and Matter
  • 22B-1. The Electromagnetic Spectrum
  • 22B-2. Spectroscopic Measurements
  • 22C. Absorption of Radiation
  • 22C-1. The Absorption Process
  • 22C-2. Absorption Spectra
  • 22C-3. Limits to Beer’s Law
  • 22D. Emission of Electromagnetic Radiation
  • 22D-1. Emission Spectra
  • 22D-2. Emission by Fluorescence and Phosphorescence
  • Chapter 22. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 23. Instruments for Optical Spectrometry
  • 23A. Instrument Components
  • 23A-1. Optical Materials
  • 23A-2. Spectroscopic Sources
  • 23A-3. Wavelength Selectors
  • 23A-4. Detecting and Measuring Radiant Energy
  • 23A-5. Signal Processors and Readout Devices
  • 23A-6. Sample Containers
  • 23B. Ultraviolet/Visible Photometers and Spectrophotometers
  • 23B-1. Single-Beam Instruments
  • 23B-2. Double-Beam Instruments
  • 23B-3. Multichannel Instruments
  • 23C. Infrared Spectrophotometers
  • 23C-1. Dispersive Infrared Instruments
  • 23C-2. Fourier Transform Instruments
  • Chapter 23. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 24. Molecular Absorption Spectrometry
  • 24A. Ultraviolet and Visible Molecular Absorption Spectroscopy
  • 24A-1. Absorbing Species
  • 24A-2. Qualitative Applications of Ultraviolet/Visible Spectroscopy
  • 24A-3. Quantitative Applications
  • 24A-4. Photometric and Spectrophotometric Titrations
  • 24A-5. Spectrophotometric Studies of Complex Ions
  • 24B. Automated Photometric and Spectrophotometric Methods
  • 24B-1. Instrumentation
  • 24B-2. A Typical Application of FIA
  • 24C. Infrared Absorption Spectroscopy
  • 24C-1. Infrared Absorption Spectra
  • 24C-2. Instruments for Infrared Spectrometry
  • 24C-3. Qualitative Applications of Infrared Spectrometry
  • 24C-4. Quantitative Infrared Spectrometry
  • Chapter 24. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 25. Molecular Fluorescence Spectroscopy
  • 25A. Theory of Molecular Fluorescence
  • 25A-1. Relaxation Processes
  • 25A-2. Fluorescent Species
  • 25B. Effect of Concentration on Fluorescence Intensity
  • 25C. Fluorescence Instrumentation
  • 25D. Applications of Fluorescence Methods
  • 25D-1. Methods for Inorganic Species
  • 25D-2. Methods for Organic and Biochemical Species
  • 25E. Molecular Phosphorescence Spectroscopy
  • 25F. Chemiluminescence Methods
  • Chapter 25. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 26. Atomic Spectroscopy
  • 26A. Origins of Atomic Spectra
  • 26A-1. Emission Spectra
  • 26A-2. Absorption Spectra
  • 26A-3. Fluorescence Spectra
  • 26A-4. Widths of Atomic Spectral Lines
  • 26B. Production of Atoms and Ions
  • 26B-1. Sample Introduction Systems
  • 26B-2. Plasma Sources
  • 26B-3. Flame Atomizers
  • 26B-4. Electrothermal Atomizers
  • 26B-5. Other Atomizers
  • 26C. Atomic Emission Spectrometry
  • 26C-1. Instrumentation
  • 26C-2. Sources of Nonlinearity in Atomic Emission Spectrometry
  • 26C-3. Interferences in Plasma and Flame Atomic Emission Spectrometry
  • 26C-4. Applications
  • 26D. Atomic Absorption Spectrometry
  • 26D-1. Line-Width Effects in Atomic Absorption
  • 26D-2. Instrumentation
  • 26D-3. Flame Atomic Absorption
  • 26D-4. Atomic Absorption with Electrothermal Atomization
  • 26D-5. Interferences in Atomic Absorption
  • 26E. Atomic Fluorescence Spectrometry
  • Chapter 26. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 27. Mass Spectrometry
  • 27A. Principles of Mass Spectrometry
  • 27A-1. Atomic Masses
  • 27A-2. Mass-to-Charge Ratio
  • 27B. Mass Spectrometers
  • 27B-1. Components of Mass Spectrometer
  • 27B-2. Mass Analyzers
  • 27B-3. Transducers for Mass Spectrometry
  • 27C. Atomic Mass Spectrometry
  • 27C-1. Sources for Atomic Mass Spectrometry
  • 27C-2. Atomic Mass Spectra and Interferences
  • 27C-3. Applications of Atomic Mass Spectrometry
  • 27D. Molecular Mass Spectrometry
  • 27D-1. Molecular Mass Spectra
  • 27D-2. Ion Sources
  • 27D-3. Molecular Mass Spectrometric Instrumentation
  • 27D-4. Applications of Molecular Mass Spectrometry
  • Chapter 27. Summary
  • Key Terms
  • Important Equation
  • Questions and Problems
  • Part VI. Kinetics and Separations
  • Chapter 28. Kinetic Methods of Analysis
  • 28A. Rates of Chemical Reactions
  • 28A-1. Reaction Mechanisms and Rate Laws
  • 28A-2. The Rate Law for First-Order Reactions
  • 28A-3. Rate Laws for Second-Order and Pseudo-First-Order Reactions
  • 28A-4. Catalyzed Reactions
  • 28B. Determining Reaction Rates
  • 28B-1. Experimental Methods
  • 28B-2. Types of Kinetic Methods
  • 28C. Applications of Kinetic Methods
  • 28C-1. Catalytic Methods
  • 28C-2. Uncatalyzed Reactions
  • 28C-3. Kinetic Determination of Components in Mixtures
  • Chapter 28. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 29. Introduction to Analytical Separations
  • 29A. Separation by Precipitation
  • 29A-1. Separations Based on Control of Acidity
  • 29A-2. Sulfide Separations
  • 29A-3. Separations by Other Inorganic Precipitants
  • 29A-4. Separations by Organic Precipitants
  • 29A-5. Separation of Species Present in Trace Amounts by Precipitation
  • 29A-6. Separation by Electrolytic Precipitation
  • 29A-7. Salt-Induced Precipitation of Proteins
  • 29B. Separation of Species by Distillation
  • 29C. Separation by Extraction
  • 29C-1. Principles
  • 29C-2. Extracting Inorganic Species
  • 29C-3. Solid-Phase Extraction
  • 29D. Separating Ions by Ion Exchange
  • 29D-1. Ion-Exchange Resins
  • 29D-2. Ion-Exchange Equilibria
  • 29D-3. Applications of Ion-Exchange Methods
  • 29E. Chromatographic Separations
  • 29E-1. General Description of Chromatography
  • 29E-2. Classification of Chromatographic Methods
  • 29E-3. Elution in Column Chromatography
  • 29E-4. Migration Rates of Solutes
  • 29E-5. Band Broadening and Column Efficiency
  • 29E-6. Variables Affecting Column Efficiency
  • 29E-7. Column Resolution
  • 29E-8. Applications of Chromatography
  • Chapter 29. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 30. Gas Chromatography
  • 30A. Instruments for Gas-Liquid Chromatography
  • 30A-1. Carrier Gas System
  • 30A-2. Sample Injection System
  • 30A-3. Column Configurations and Column Ovens
  • 30A-4. Chromatographic Detectors
  • 30B. Gas Chromatographic Columns and Stationary Phases
  • 30B-1. Capillary Columns
  • 30B-2. Packed Columns
  • 30B-3. Liquid Stationary Phases
  • 30C. Applications of Gas-Liquid Chromatography
  • 30C-1. Qualitative Analysis
  • 30C-2. Quantitative Analysis
  • 30C-3. Advances in GC
  • 30D. Gas-Solid Chromatography
  • Chapter 30. Summary
  • Key Terms
  • Important Equations
  • Questions and Problems
  • Chapter 31. High-Performance Liquid Chromatography
  • 31A. Instrumentation
  • 31A-1. Mobile-Phase Reservoirs and Solvent Treatment Systems
  • 31A-2. Pumping Systems
  • 31A-3. Sample Injection Systems
  • 31A-4. Columns for HPLC
  • 31A-5. HPLC Detectors
  • 31B. Partition Chromatography
  • 31B-1. Bonded-Phase Packings
  • 31B-2. Normal- and Reversed-Phase Packings
  • 31B-3. Choice of Mobile and Stationary Phases
  • 31B-4. Applications
  • 31C. Adsorption Chromatography
  • 31D. Ion Chromatography
  • 31D-1. Ion Chromatography Based on Suppressors
  • 31D-2. Single-Column Ion Chromatography
  • 31E. Size-Exclusion Chromatography
  • 31E-1. Column Packings
  • 31E-2. Applications
  • 31F. Affinity Chromatography
  • 31G. Chiral Chromatography
  • 31H. Comparison of High-Performance Liquid Chromatography and Gas Chromatography
  • Chapter 31. Summary
  • Key Terms
  • Questions and Problems
  • Chapter 32. Miscellaneous Separation Methods
  • 32A. Supercritical Fluid Separations
  • 32A-1. Properties of Supercritical Fluids
  • 32A-2. Instrumentation and Operating Variables
  • 32A-3. Supercritical Fluid Chromatography versus Other Column Methods
  • 32A-4. Applications
  • 32B. Planar Chromatography
  • 32B-1. The Scope of Thin-Layer Chromatography
  • 32B-2. Principles of Thin-Layer Chromatography
  • 32B-3. Paper Chromatography
  • 32C. Capillary Electrophoresis
  • 32C-1. Instrumentation for Capillary Electrophoresis
  • 32C-2. Electroosmotic Flow
  • 32C-3. The Basis for Electrophoretic Separations
  • 32C-4. Applications of Capillary Electrophoresis
  • 32D. Capillary Electrochromatography
  • 32D-1. Packed Column Electrochromatography
  • 32D-2. Micellar Electrokinetic Capillary Chromatography
  • 32E. Field-Flow Fractionation
  • 32E-1. Separation Mechanisms
  • 32E-2. FFF Methods
  • 32E-3. Advantages of FFF over Chromatographic Methods
  • Chapter 32. Summary
  • Key Terms
  • Questions and Problems
  • Part VII. Practical Aspects of Chemical Analysis
  • Chapter 33. The Analysis of Real Samples
  • 33A. Real Samples
  • 33B. Choice of Analytical Method
  • 33B-1. Definition of the Problem
  • 33B-2. Investigating the Literature
  • 33B-3. Choosing or Devising a Method
  • 33B-4. Testing the Procedure
  • 33C. Accuracy in the Analysis of Complex Materials
  • Chapter 34. Preparing Samples for Analysis
  • 34A. Preparing Laboratory Samples
  • 34A-1. Crushing and Grinding Samples
  • 34A-2. Mixing Solid Samples
  • 34B. Moisture in Samples
  • 34B-1. Forms of Water in Solids
  • 34B-2. Temperature and Humidity Effects on the Water Content of Solids
  • 34B-3. Drying the Analytical Sample
  • 34C. Determining Water in Samples
  • Chapter 35. Decomposing and Dissolving the Sample
  • 35A. Sources of Error in Decomposition and Dissolution
  • 35B. Decomposing Samples with Inorganic Acids in Open Vessels
  • 35B-1. Hydrochloric Acid
  • 35B-2. Nitric Acid
  • 35B-3. Sulfuric Acid
  • 35B-4. Perchloric Acid
  • 35B-5. Oxidizing Mixtures
  • 35B-6. Hydrofluoric Acid
  • 35C. Microwave Decompositions
  • 35C-1. Vessels for Moderate-Pressure Digestions
  • 35C-2. High-Pressure Microwave Vessels
  • 35C-3. Atmospheric-Pressure Digestions
  • 35C-4. Microwave Ovens
  • 35C-5. Microwave Furnaces
  • 35C-6. Applications of Microwave Decompositions
  • 35D. Combustion Methods for Decomposing Organic Samples
  • 35D-1. Combustion over an Open Flame (Dry Ashing)
  • 35D-2. Combustion-Tube Methods
  • 35D-3. Combustion with Oxygen in a Sealed Container
  • 35E. Decomposing Inorganic Materials with Fluxes
  • 35E-1. Fusion Procedure
  • 35E-2. Types of Fluxes
  • Chapter 36. Chemicals, Apparatus, and Unit Operations of Analytical Chemistry
  • 36A. Selecting and Handling Reagents and Other Chemicals
  • 36A-1. Classifying Chemicals
  • 36A-2. Rules for Handling Reagents and Solutions
  • 36B. Cleaning and Marking of Laboratory Ware
  • 36C. Evaporating Liquids
  • 36D. Measuring Mass
  • 36D-1. Types of Analytical Balances
  • 36D-2. The Electronic Analytical Balance
  • 36D-3. The Single-Pan Mechanical Analytical Balance
  • 36D-4. Sources of Error in Weighing
  • 36D-5. Auxiliary Balances
  • 36E. Equipment and Manipulations Associated with Weighing
  • 36E-1. Weighing Bottles
  • 36E-2. Desiccators and Desiccants
  • 36E-3. Manipulating Weighing Bottles
  • 36E-4. Weighing by Difference
  • 36E-5. Weighing Hygroscopic Solids
  • 36E-6. Weighing Liquids
  • 36F. Filtration and Ignition of Solids
  • 36F-1. Apparatus
  • 36F-2. Filtering and Igniting Precipitates
  • 36F-3. Directions for Filtering and Igniting Precipitates
  • 36F-4. Rules for Manipulating Heated Objects
  • 36G. Measuring Volume
  • 36G-1. Units of Volume
  • 36G-2. The Effect of Temperature on Volume Measurements
  • 36G-3. Apparatus for Precisely Measuring Volume
  • 36G-4. Using Volumetric Equipment
  • 36G-5. Directions for Using a Pipet
  • 36G-6. Directions for Using a Buret
  • 36G-7. Directions for Using a Volumetric Flask
  • 36H. Calibrating Volumetric Glassware
  • 36H-1. General Directions for Calibration
  • 36I. The Laboratory Notebook
  • 36I-1. Maintaining a Laboratory Notebook
  • 36I-2. Notebook Format
  • 36J. Safety in the Laboratory
  • Chapter 37. Selected Methods of Analysis
  • 37A. An Introductory Experiment
  • 37A-1. Using the Analytical Balance
  • 37A-2. Making Quantitative Transfers
  • 37A-3. Delivering an Aliquot
  • 37A-4. Calibrating a Pipet
  • 37A-5. Reading Buret Sections
  • 37A-6. Reading a Buret
  • 37A-7. Sampling
  • 37A-8. Determining Sampling Error by Flow Injection Analysis
  • 37B. Gravimetric Methods of Analysis
  • 37B-1. The Gravimetric Determination of Chloride in a Soluble Sample
  • 37B-2. The Gravimetric Determination of Tin in Brass
  • 37B-3. The Gravimetric Determination of Nickel in Steel
  • 37C. Neutralization Titrations
  • Discussion
  • 37C-1. The Effect of Atmospheric Carbon Dioxide on Neutralization Titrations
  • 37C-2. Preparation of Indicator Solutions for Neutralization Titrations
  • 37C-3. Preparation of Dilute Hydrochloric Acid Solutions
  • 37C-4. Preparation of Carbonate-Free Sodium Hydroxide
  • 37C-5. The Determination of the Acid/Base Ratio
  • 37C-6. Standardization of Hydrochloric Acid against Sodium Carbonate
  • 37C-7. Standardization of Sodium Hydroxide against Potassium Hydrogen Phthalate
  • 37C-8. The Determination of Potassium Hydrogen Phthalate in an Impure Sample
  • 37C-9. Determining the Acid Content of Vinegars and Wines
  • 37C-10. The Determination of Sodium Carbonate in an Impure Sample
  • 37C-11. The Determination of Amine Nitrogen by the Kjeldahl Method
  • 37D. Precipitation Titrations
  • 37D-1. Preparing a Standard Silver Nitrate Solution
  • 37D-2. The Determination of Chloride by Titration with an Adsorption Indicator
  • 37D-3. The Determination of Chloride by a Weight Titration
  • 37E. Complex-Formation Titrations with EDTA
  • 37E-1. Preparation of Solutions
  • 37E-2. Preparation of Standard 0.01 ⁢ M EDTA Solution
  • 37E-3. The Determination of Magnesium by Direct Titration
  • 37E-4. The Determination of Calcium by Displacement Titration
  • 37E-5. The Determination of Hardness in Water
  • 37F. Titrations with Potassium Permanganate
  • 37F-1. Preparation of 0.02 ⁢ M Potassium Permanganate
  • 37F-2. Standardization of Potassium Permanganate Solutions
  • 37F-3. The Determination of Calcium in a Limestone
  • 37F-4. The Determination of Iron in an Ore
  • 37G. Titrations with Iodine
  • 37G-1. Preparation of Reagents
  • 37G-2. Standardization of Iodine Solutions
  • 37G-3. The Determination of Antimony in Stibnite
  • 37H. Titrations with Sodium Thiosulfate
  • 37H-1. Preparation of 0.1 ⁢ M Sodium Thiosulfate
  • 37H-2. Standardization of Sodium Thiosulfate against Potassium Iodate
  • 37H-3. Standardization of Sodium Thiosulfate against Copper
  • 37H-4. The Determination of Copper in Brass
  • 37I. Titrations with Potassium Bromate
  • 37I-1. Preparation of Solutions
  • 37I-2. Standardization of Sodium Thiosulfate against Potassium Bromate
  • 37I-3. The Determination of Ascorbic Acid in Vitamin C Tablets by Titration with Potassium Bromate
  • 37J. Potentiometric Methods
  • 37J-1. General Directions for Performing a Potentiometric Titration
  • 37J-2. Potentiometric Titration of Chloride and Iodide in a Mixture
  • 37J-3. The Potentiometric Determination of Solute Species in a Carbonate Mixture
  • 37J-4. The Direct Potentiometric Determination of Fluoride Ion
  • 37K. Electrogravimetric Methods
  • 37K-1. The Electrogravimetric Determination of Copper and Lead in Brass
  • 37L. Coulometric Titrations
  • 37L-1. The Coulometric Titration of Cyclohexene
  • 37M. Voltammetry
  • 37M-1. The Polarographic Determination of Copper and Zinc in Brass
  • 37M-2. The Amperometric Titration of Lead
  • 37N. Methods Based on the Absorption of Radiation
  • 37N-1. The Cleaning and Handling of Cells
  • 37N-2. The Determination of Iron in a Natural Water
  • 37N-3. The Determination of Manganese in Steel
  • 37N-4. The Spectrophotometric Determination of pH
  • 37O. Molecular Fluorescence
  • 37O-1. The Determination of Quinine in Beverages
  • 37P. Atomic Spectroscopy
  • 37P-1. The Determination of Lead in Brass by Atomic Absorption Spectroscopy
  • 37P-2. The Determination of Sodium, Potassium, and Calcium in Mineral Waters by Atomic Emission Spectroscopy
  • 37Q. Application of Ion-Exchange Resins
  • 37Q-1. The Separation of Cations
  • 37Q-2. Determination of Magnesium by Ion-Exchange Chromatography
  • 37R. Gas-Liquid Chromatography
  • 37R-1. The Gas Chromatographic Determination of Ethanol in Beverages
  • Appendix 1. The Literature of Analytical Chemistry
  • Appendix 2. Solubility Product Constants at 25 C °
  • Appendix 3. Acid Dissociation Constants at 25 C °
  • Appendix 4. Formation Constants at 25 C °
  • Appendix 5. Standard and Formal Electrode Potentials
  • Appendix 6. Use of Exponential Numbers and Logarithms
  • Appendix 7. Volumetric Calculations Using Normality and Equivalent Weight
  • Appendix 8. Compounds Recommended for the Preparation of Standard Solutions of Some Common Elements
  • Appendix 9. Derivation of Error Propagation Equations