Modern Analytical Chemistry

Автор(ы):Harvey D.
06.10.2007
Год изд.:2000
Описание: Chemistry is the study of matter, including its composition, structure, physical properties, and reactivity. There are many approaches to studying chemistry, but, for convenience, we traditionally divide it into five fields: organic, inorganic, physical, biochemical, and analytical. Although this division is historical and arbitrary, as witnessed by the current interest in interdisciplinary areas such as bioanalytical and organometallic chemistry, these five fields remain the simplest division spanning the discipline of chemistry. Training in each of these fields provides a unique perspective to the study of chemistry. Undergraduate chemistry courses and textbooks are more than a collection of facts; they are a kind of apprenticeship. In keeping with this spirit, this text introduces the field of analytical chemistry and the unique perspectives that analytical chemists bring to the study of chemistry. Книга повествует о современной аналитической химии - точнее, о той ее версии, которой придерживается автор.
Оглавление:
Modern Analytical Chemistry — обложка книги. Обложка книги.
Chapter I Introduction [1]
  1A What is Analytical Chemistry? [2]
  1B The Analytical Perspective [5]
  1C Common Analytical Problems [8]
  1D Key Terms [9]
  1E Summary [9]
  1F Problems [9]
  1G Suggested Readings [10]
  1H References [10]
Chapter 2 Basic Tools of Analytical Chemistry [11]
  2A Numbers in Analytical Chemistry [12]
    2A.1 Fundamental Units of Measure [12]
    2A.2 Significant Figures [13]
  2B Units for Expressing Concentration [15]
    2B.1 Molarity and Formality [15]
    2B.2 Normality [16]
    2B.3 Molality [18]
    2B.4 Weight, Volume, and Weight-to-Volume Ratios [18]
    2B.5 Converting Between Concentration Units [18]
    2B.6 p-Functions [19]
  2C Stoichiometric Calculations [20]
    2C.1 Conservation of Mass [22]
    2C.2 Conservation of Charge [22]
    2C.3 Conservation of Protons [22]
    2C.4 Conservation of Electron Pairs [23]
    2C.5 Conservation of Electrons [23]
    2C.6 Using Conservation Principles in Stoichiometry Problems [23]
  2D Basic Equipment and Instrumentation [25]
    2D.1 Instrumentation for Measuring Mass [25]
    2D.2 Equipment for Measuring Volume [26]
    2D.3 Equipment for Drying Samples [29]
  2E Preparing Solutions [30]
    2E.1 Preparing Stock Solutions [30]
    2E.2 Preparing Solutions by Dilution [31]
  2F The Laboratory Notebook [32]
  2G Key Terms [32]
  2H Summary [33]
  2I Problems [33]
  2J Suggested Readings [34]
  2K References [34]
Chapter 3 The Language of Analytical Chemistry [35]
  ЗА Analysis, Determination, and Measurement [36]
  3B Techniques, Methods, Procedures, and Protocols [36]
  3C Classifying Analytical Techniques [37]
  3D Selecting an Analytical Method [38]
    3D.1 Accuracy [38]
    3D.2 Precision [39]
    3D.3 Sensitivity [39]
    3D.4 Selectivity [40]
    3D.5 Robustness and Ruggedness [42]
    3D.6 Scale of Operation [42]
    3D.7 Equipment, Time, and Cost [44]
    3D.8 Making the Final Choice [44]
  3Е Developing the Procedure [45]
    3E.1 Compensating for Interferences [45]
    3E.2 Calibration and Standardization [47]
    3E.3 Sampling [47]
    3E.4 Validation [47]
  3F Protocols [48]
  3G The Importance of Analytical Methodology [48]
  3H Key Terms [50]
  3I Summary [50]
  3J Problems [51]
  3K Suggested Readings [52]
  3L References [52]
Chapter 4 Evaluating Analytical Data [53]
  4A Characterizing Measurements and Results [54]
    4A.1 Measures of Central Tendency [54]
    4A.2 Measures of Spread [55]
  4B Characterizing Experimental Errors [57]
    4B.1 Accuracy [57]
    4B.2 Precision [62]
    4B.3 Error and Uncertainty [64]
  4C Propagation of Uncertainty [64]
    4C.1 A Few Symbols [65]
    4C.2 Uncertainty When Adding or Subtracting [65]
    4C.3 Uncertainty When Multiplying or Dividing [66]
    4C.4 Uncertainty for Mixed Operations [66]
    4C.5 Uncertainty for Other Mathematical Functions [67]
    4C.6 Is Calculating Uncertainty Actually Useful? [68]
  4D The Distribution of Measurements and Results [70]
    4D.1 Populations and Samples [71]
    4D.2 Probability Distributions for Populations [71]
    4D.3 Confidence Intervals for Populations [75]
    4D.4 Probability Distributions for Samples [77]
    4D.5 Confidence Intervals for Samples [80]
    4D.6 A Cautionary Statement [81]
  4E Statistical Analysis of Data [82]
    4E.1 Significance Testing [82]
    4E.2 Constructing a Significance Test [83]
    4E.3 One-Tailed and Two-Tailed Significance Tests [84]
    4E.4 Errors in Significance Testing [84]
  4F Statistical Methods for Normal Distributions [85]
    4F.1 Comparing (?) to (?) [85]
    4F.2 Comparing (?) to (?) [87]
    4F.3 Comparing Two Sample Variances [88]
    4F.4 Comparing Two Sample Means [88]
    4F.5 Outliers [93]
  4G Detection Limits [95]
  4H Key Terms [96]
  4I Summary [96]
  4J Suggested Experiments [97]
  4K Problems [98]
  4L Suggested Readings [102]
  4M References [102]
Chapter 5 Calibrations, Standardizations, and Blank Corrections [104]
  5A Calibrating Signals [105]
  5B Standardizing Methods [106]
    5B.1 Reagents Used as Standards [106]
    5B.2 Single-Point versus Multiple-Point Standardizations [108]
    5B.3 External Standards [109]
    5B.4 Standard Additions [110]
    5B.5 Internal Standards [115]
  5C Linear Regression and Calibration Curves [117]
    5C.1 Linear Regression of Straight-Line Calibration Curves [118]
    5C.2 Unweighted Linear Regression with Errors iny [119]
    5C.3 Weighted Linear Regression with Errors in у [124]
    5C.4 Weighted Linear Regression with Errors in Both x and у [127]
    5C.5 Curvilinear and Multivariate Regression [127]
  5D Blank Corrections [128]
  5E Key Terms [130]
  5F Summary [130]
  5G Suggested Experiments [130]
  5H Problems [131]
  5I Suggested Readings [133]
  5J References [134]
Chapter 6 Equilibrium Chemistry [135]
  6A Reversible Reactions and Chemical Equilibria [136]
  6B Thermodynamics and Equilibrium Chemistry [136]
  6C Manipulating Equilibrium Constants [138]
  6D Equilibrium Constants for Chemical Reactions [139]
    6D.1 Precipitation Reactions [139]
    6D.2 Acid-Base Reactions [140]
    6D.3 Complexation Reactions [144]
    6D.4 Oxidation-Reduction Reactions [145]
  6E Le Chatelier's Principle [148]
  6F Ladder Diagrams [150]
    6F.1 Ladder Diagrams for Acid-Base Equilibria [150]
    6F.2 Ladder Diagrams for Complexation Equilibria [153]
    6F.3 Ladder Diagrams for Oxidation-Reduction Equilibria [155]
  6G Solving Equilibrium Problems [156]
    6G.1 A Simple Problem: Solubility of Pb (IO3) 2 in Water [156]
    6G.2 A More Complex Problem: The Common Ion Effect [157]
    6G.3 Systematic Approach to Solving Equilibrium Problems [159]
    6G.4 pH of a Monoprotic Weak Acid [160]
    6G.5 pH of a Polyprotic Acid or Base [163]
    6G.6 Effect of Complexation on Solubility [165]
  6H Buffer Solutions [167]
    6H.1 Systematic Solution to Buffer Problems [168]
    6H.2 Representing Buffer Solutions with Ladder Diagrams [170]
  6I Activity Effects [171]
  6J Two Final Thoughts About Equilibrium Chemistry [175]
  6K Key Terms [175]
  6L Summary [175]
  6M Suggested Experiments [176]
  6N Problems [176]
  6O Suggested Readings [178]
  6P References [178]
Chapter 7 Obtaining and Preparing Samples for Analysis [179]
  7A The Importance of Sampling [180]
  7B Designing a Sampling Plan [182]
    7B.1 Where to Sample the Target Population [182]
    7B.2 What Type of Sample to Collect [185]
    7B.3 How Much Sample to Collect [187]
    7B.4 How Many Samples to Collect [191]
    7B.5 Minimizing the Overall Variance [192]
  7C Implementing the Sampling Plan [193]
    7C.1 Solutions [193]
    7C.2 Gases [195]
    7C.3 Solids [196]
  7D Separating the Analyte from Interferents [201]
  7E General Theory of Separation Efficiency [202]
  7F Classifying Separation Techniques [205]
    7F.1 Separations Based on Size [205]
    7F.2 Separations Based on Mass or Density [206]
    7F.3 Separations Based on Complexation Reactions (Masking) [207]
    7F.4 Separations Based on a Change of State [209]
    7F.5 Separations Based on a Partitioning Between Phases [211]
  7G Liquid-Liquid Extractions [215]
    7G.1 Partition Coefficients and Distribution Ratios [216]
    7G.2 Liquid-Liquid Extraction with No Secondary Reactions [216]
    7G.3 Liquid-Liquid Extractions Involving Acid-Base Equilibria [219]
    7G.4 Liquid-Liquid Extractions Involving Metal Chelators [221]
  7H Separation versus Preconcentration [223]
  7I Key Terms [224]
  7J Summary [224]
  7K Suggested Experiments [225]
  7L Problems [226]
  7M Suggested Readings [230]
  7N References [231]
Chapter 8 Gravimetric Methods of Analysis [232]
  8A Overview of Gravimetry [233]
    8A.1 Using Mass as a Signal [233]
    8A.2 Types of Gravimetric Methods [234]
    8A.3 Conservation of Mass [234]
    8A.4 Why Gravimetry Is Important [235]
  8B Precipitation Gravimetry [235]
    8B.1 Theory and Practice [235]
    8B.2 Quantitative Applications [247]
    8B.3 Qualitative Applications [254]
    8B.4 Evaluating Precipitation Gravimetry [254]
  8C Volatilization Gravimetry [255]
    8C.1 Theory and Practice [255]
    8C.2 Quantitative Applications [259]
    8C.3 Evaluating Volatilization Gravimetry [262]
  8D Particulate Gravimetry [262]
    8D.1 Theory and Practice [263]
    8D.2 Quantitative Applications [264]
    8D.3 Evaluating Precipitation Gravimetry [265]
  8E Key Terms [265]
  8F Summary [266]
  8G Suggested Experiments [266]
  8H Problems [267]
  8I Suggested Readings [271]
  8J References [272]
Chapter 9 Titrimetric Methods of Analysis [273]
  9A Overview of Titrimetry [274]
    9A.1 Equivalence Points and End Points [274]
    9A.2 Volume as a Signal [274]
    9A.3 Titration Curves [275]
    9A.4 The Buret [277]
  9B Titrations Based on Acid-Base Reactions [278]
    9B.1 Acid-Base Titration Curves [279]
    9B.2 Selecting and Evaluating the End Point [287]
    9B.3 Titrations in Nonaqueous Solvents [295]
    9B.4 Representative Method [296]
    9B.5 Quantitative Applications [298]
    9B.6 Qualitative Applications [308]
    9B.7 Characterization Applications [309]
    9B.8 Evaluation of Acid-Base Titrimetry [311]
  9C Titrations Based on Complexation Reactions [314]
    9C.1 Chemistry and Properties of EDTA [315]
    9C.2 Complexometric EDTA Titration Curves [317]
    9C.3 Selecting and Evaluating the End Point [322]
    9C.4 Representative Method [324]
    9C.5 Quantitative Applications [327]
    9C.6 Evaluation of Complexation Titrimetry [331]
  9D Titrations Based on Redox Reactions [331]
    9D.1 Redox Titration Curves [332]
    9D.2 Selecting and Evaluating the End Point [337]
    9D.3 Representative Method [340]
    9D.4 Quantitative Applications [341]
    9D.5 Evaluation of Redox Titrimetry [350]
  9E Precipitation Titrations [350]
    9E.1 Titration Curves [350]
    9E.2 Selecting and Evaluating the End Point [354]
    9E.3 Quantitative Applications [354]
    9E.4 Evaluation of Precipitation Titrimetry [357]
  9F Key Terms [357]
  9G Summary [357]
  9H Suggested Experiments [358]
  9I Problems [360]
  9J Suggested Readings [366]
  9K References [367]
Chapter 10 Spectroscopic Methods oj Analysis [368]
  10A Overview of Spectroscopy [369]
    10A.1 What Is Electromagnetic Radiation [369]
    10A.2 Measuring Photons as a Signal [372]
  10B Basic Components of Spectroscopic Instrumentation [374]
    10B.1 Sources of Energy [375]
    10B.2 Wavelength Selection [376]
    10B.3 Detectors [379]
    10B.4 Signal Processors [380]
  10C Spectroscopy Based on Absorption [380]
    10C.1 Absorbance of Electromagnetic Radiation [380]
    10C.2 Transmittance and Absorbance [384]
    10C.3 Absorbance and Concentration: Beer's Law [385]
    10С.4 Beer's Law and Multicomponent Samples [386]
    10C.5 Limitations to Beer's Law [386]
  10D Ultraviolet-Visible and Infrared Spectrophotometry [388]
    10D.1 Instrumentation [388]
    10D.2 Quantitative Applications [394]
    10D.3 Qualitative Applications [402]
    10D.4 Characterization Applications [403]
    10D.5 Evaluation [409]
  10E Atomic Absorption Spectroscopy [412]
    10E.1 Instrumentation [412]
    10E.2 Quantitative Applications [415]
    10E.3 Evaluation [422]
  10F Spectroscopy Based on Emission [423]
  10G Molecular Photoluminescence Spectroscopy [423]
    10G.1 Molecular Fluorescence and Phosphorescence Spectra [424]
    10G.2 Instrumentation [427]
    10G.3 Quantitative Applications Using Molecular Luminescence [429]
    10G.4 Evaluation [432]
  10H Atomic Emission Spectroscopy [434]
    10H.1 Atomic Emission Spectra [434]
    10H.2 Equipment [435]
    10H.3 Quantitative Applications [437]
    10H.4 Evaluation [440]
  10I Spectroscopy Based on Scattering [441]
    10I.1 Origin of Scattering [441]
    10I.2 Turbidimetry and Nephelometry [441]
  10J Key Terms [446]
  10K Summary [446]
  10L Suggested Experiments [447]
  10M Problems [450]
  10N Suggested Readings [458]
  10O References [459]
Chapter 11 Electrochemical Methods of Analysis [461]
  11A Classification of Electrochemical Methods [462]
    11A.1 Interfacial Electrochemical Methods [462]
    11A.2 Controlling and Measuring Current and Potential [462]
  11B Potentiometric Methods of Analysis [465]
    11B.1 Potentiometric Measurements [466]
    11B.2 Reference Electrodes [471]
    11B.3 Metallic Indicator Electrodes [473]
    11B.4 Membrane Electrodes [475]
    11B.5 Quantitative Applications [485]
    11B.6 Evaluation [494]
  11C Coulometric Methods of Analysis [496]
    11C.1 Controlled-Potential Coulometry [497]
    11C.2 Controlled-Current Coulometry [499]
    11C.3 Quantitative Applications [501]
    11C.4 Characterization Applications [506]
    11C.5 Evaluation [507]
  11D Voltammetric Methods of Analysis [508]
    11D.1 Voltammetric Measurements [509]
    11D.2 Current in Voltammetry [510]
    11D.3 Shape of Voltammograms [513]
    11D.4 Quantitative and Qualitative Aspects of Voltammetry [514]
    11D.5 Voltammetric Techniques [515]
    11D.6 Quantitative Applications [520]
    11D.7 Characterization Applications [527]
    11D.8 Evaluation [531]
  11E Key Terms [532]
  11F Summary [532]
  11G Suggested Experiments [533]
  11H Problems [535]
  11I Suggested Readings [540]
  11J References [541]
Chapter 12 Chromatographic and Electrophoretic Methods [543]
  12A Overview of Analytical Separations [544]
    12A.1 The Problem with Simple Separations [544]
    12A.2 A Better Way to Separate Mixtures [544]
    12A.3 Classifying Analytical Separations [546]
  12B General Theory of Column Chromatography [547]
    12B.1 Chromatographic Resolution [549]
    12B.2 Capacity Factor [550]
    12B.3 Column Selectivity [552]
    12B.4 Column Efficiency [552]
    12В.5 Peak Capacity [554]
    12B.6 Nonideal Behavior [555]
  12C Optimizing Chromatographic Separations [556]
    12C.1 Using the Capacity Factor to Optimize Resolution [556]
    12C.2 Using Column Selectivity to Optimize Resolution [558]
    12C.3 Using Column Efficiency to Optimize Resolution [559]
  12D Gas Chromatography [563]
    12D.1 Mobile Phase [563]
    12D.2 Chromatographic Columns [564]
    12D.3 Stationary Phases [565]
    12D.4 Sample Introduction [567]
    12D.5 Temperature Control [568
    12D.6 Detectors for Gas Chromatography [569]
    12D.7 Quantitative Applications [571]
    12D.8 Qualitative Applications [575]
    12D.9 Representative Method [576]
    12D.10 Evaluation [577]
  12E High-Performance Liquid Chromatography [578]
    12E.1 HPLC Columns [578]
    12E.2 Stationary Phases [579]
    12E.3 Mobile Phases [580]
    12E.4 HPLC Plumbing [583]
    12E.5 Sample Introduction [584]
    12E.6 Detectors for HPLC [584]
    12E.7 Quantitative Applications [586]
    12E.8 Representative Method [588]
    12E.9 Evaluation [589]
  12F Liquid-Solid Adsorption Chromatography [590]
  12G Ion-Exchange Chromatography [590]
  12H Size-Exclusion Chromatography [593]
  12I Supercritical Fluid Chromatography [596]
  12J Electrophoresis [597]
    12J.1 Theory of Capillary Electrophoresis [598]
    12J.2 Instrumentation [601]
    12J.3 Capillary Electrophoresis Methods [604]
    12J.4 Representative Method [607]
    12J.5 Evaluation [609]
  12K Key Terms [609]
  12L Summary [610]
  12M Suggested Experiments [610]
  12N Problems [615]
  12O Suggested Readings [620]
  12P References [620]
Chapter 13 Kinetic Methods of Analysis [622]
  13A Methods Based on Chemical Kinetics [623]
    13A.1 Theory and Practice [624]
    13A.2 Instrumentation [634]
    13A.3 Quantitative Applications [636]
    13A.4 Characterization Applications [638]
    13A.5 Evaluation of Chemical Kinetic Methods [639]
  13B Radiochemical Methods of Analysis [642]
    13B.1 Theory and Practice [643]
    13B.2 Instrumentation [643]
    13B.3 Quantitative Applications [644]
    13B.4 Characterization Applications [647]
    13B.5 Evaluation [648]
  13C Flow Injection Analysis [649]
    13C.1 Theory and Practice [649]
    13C.2 Instrumentation [651]
    13C.3 Quantitative Applications [655]
    13C.4 Evaluation [658]
  13D Key Terms [658]
  13E Summary [659]
  13F Suggested Experiments [659]
  13G Problems [661]
  13H Suggested Readings [664]
  13I References [665]
Chapter 14 Developing a Standard Method [666]
  14A Optimizing the Experimental Procedure [667]
    14A.1 Response Surfaces [667]
    14A.2 Searching Algorithms for Response Surfaces [668]
    14A.3 Mathematical Models of Response Surfaces [674]
  14B Verifying the Method [683]
    14B.1 Single-Operator Characteristics [683]
    14B.2 Blind Analysis of Standard Samples [683]
    14B.3 Ruggedness Testing [684]
    14B.4 Equivalency Testing [687]
  14С Validating the Method as a Standard Method [687]
    14C.1 Two-Sample Collaborative Testing [688]
    14C.2 Collaborative Testing and Analysis of Variance [693]
    14C.3 What Is a Reasonable Result for a Collaborative Study? [698]
  14D Key Terms [699]
  14E Summary [699]
  14F Suggested Experiments [699]
  14G Problems [700]
  14H Suggested Readings [704]
  14I References [704]
Chapter 15 Quality Assurance [705]
  15A Quality Control [706]
  15B Quality Assessment [708]
    15B.1 Internal Methods of Quality Assessment [708]
    15B.2 External Methods of Quality Assessment [711]
  15C Evaluating Quality Assurance Data [712]
    15C.1 Prescriptive Approach [712]
    15C.2 Performance-Based Approach [714]
  15D Key Terms [721]
  15E Summary [722]
  15F Suggested Experiments [722]
  15G Problems [722]
  15H Suggested Readings [724]
  15I References [724]
Appendixes
    Appendix 1A Single-Sided Normal Distribution [725]
    Appendix 1B t-Table [726]
    Appendix 1C F-Table [727]
    Appendix 1D Critical Values for Q-Test [728]
    Appendix 1E Random Number Table [728]
  Appendix 2 Recommended Reagents for Preparing Primary Standards [729]
    Appendix 3А Solubility Products [731]
    Appendix 3B Acid Dissociation Constants [732]
    Appendix 3C Metal-Ligand Formation Constants [739]
    Appendix 3D Standard Reduction Potentials [743]
    Appendix 3E Selected Polarographic Half-Wave Potentials [747]
  Appendix 4 Balancing Redox Reactions [748]
  Appendix 5 Review of Chemical Kinetics [750]
  Appendix 6 Countercurrent Separations [755]
  Appendix 7 Answers to Selected Problems [762]
Glossary [769]
Index [781]
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