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9780471893035

Chemistry Experiments for Instrumental Methods

by ; ;
  • ISBN13:

    9780471893035

  • ISBN10:

    047189303X

  • Edition: 1st
  • Format: Paperback
  • Copyright: 1991-01-16
  • Publisher: Wiley

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Summary

The only self-contained modern laboratory manual for advanced undergraduate courses in instrumental analysis. Consists of over 50 experiments demonstrating the theory and practice of electrochemical methods, methods based on electromagnetic radiation, and separation methods. Experiments are introduced with a review of the physical principles on which the experimental procedures are based.

Author Biography

DONALD T. SAWYER is Distinguished Professor of Chemistry at Texas A&M University, and from 1956 to 1986 was on the faculty of the University of California, Riverside. Professor Sawyer is the author of 300 research publications and coauthor of ten books, including Experimental Electrochemistry for Chemists, and Electrochemical Studies of Biological Systems. His numerous awards and appointments include election as a Fellow of the American Association for the Advancement of Science; Guggenheim, Merton College, and JSPS Fellowships; and the Richard C. Tolman Medal.

Table of Contents

Preface xiii
Chapter 1 / Introduction and Bibliography
1(6)
Part 1 Electrochemical Methods 7(154)
Chapter 2 / Potentiometric Methods
9(49)
Experiment 2-1 pH Titration of H(3)PO(4) Mixtures; Calculation of K(1), K(2), and K(3)
24(4)
Experiment 2-2 Potentiometric Titration of a Chloride-Iodide Mixture; Calculation of K(sp) for AgCl and AgI Supplementary Experiments:
28(5)
I Titration of Chloride and Iodide with Permanganate
31(1)
II Determination of Chloride in Mouthwash
32(1)
Experiment 2-3 Effect of Complex Formation on the Titration of Fe^2+
33(3)
Experiment 2-4 Acid-Base Titrations in Nonaqueous Media: Titrations of Nicotine
36(6)
Experiment 2-5 Ion-Selective Electrodes Supplementary Experiments:
42(10)
I Sodium Electrode
50(1)
II Fluoride Electrode
50(1)
III Nitrate Electrode
51(1)
Experiment 2-6 Determination of the Copper(II) Ethylenediamine Stability Constants by pH Titration
52(6)
Chapter 3 / Conductometric Methods
58(14)
Experiment 3-1 Conductometric Titrations of HCl and HOAc with NaOH; Determination of K(a) for Acetic Acid Supplementary Experiments:
63(6)
I Titration of Mixed Acids with Strong Base
65(2)
II Titration of a Salt of a Weak Acid with a Strong Acid
67(1)
III A Titration Involving a Neutralization and a Precipitation
67(1)
IV Analysis of Aspirin Tablets
68(1)
Experiment 3-2 Conductometric Measurement of the Solubility of a Relatively Insoluble Compound
69(3)
Chapter 4 / Controlled Potential Methods (Voltammetry)
72(72)
Experiment 4-1 Cyclic Voltammetry
79(6)
Experiment 4-2 Study of Electrode Mechanism by Cyclic Voltammetry
85(5)
Experiment 4-3 Cyclic Voltammetry of O(2) and SO(2) in Aprotic Media
90(5)
Experiment 4-4 Polarography
95(9)
Experiment 4-5 Differential Pulse Polarography
104(4)
Experiment 4-6 Polarography of Organic Compounds: Nitrobenzene
108(2)
Experiment 4-7 Determination of the Formula and Formation Constant of a Complex Metal Ion by Polarography or Pulse Polarography
110(4)
Experiment 4-8 Anodic Stripping Voltammetry
114(5)
Experiment 4-9 Spectroelectrochemistry and Thin-Layer Cells
119(7)
Experiment 4-10 Amperometric Titrations with Dropping Mercury Electrode
126(6)
Experiment 4-11 Amperometric Titrations with Rotating Platinum Electrode
132(2)
Experiment 4-12 End-Point Detection with Dual Polarized Electrodes
134(6)
Experiment 4-13 Glucose Determination with an Immobilized Enzyme Electrode
140(4)
Chapter 5 / Electrolytic Methods and Controlled-Current Methods
144(17)
Experiment 5-1 Electrogravimetric Analysis of a Copper-Nickel Mixture
148(2)
Supplementary Experiment: Electrogravimetric Determination of Copper in Brass and Copper Ore
150(1)
Experiment 5-2 Constant-Current Coulometry: Titration of Arsenic
151(4)
Experiment 5-3 Chronopotentiometry
155(6)
Part 2 Methods Based on Electromagnetic Radiation 161(158)
Chapter 6 / Analytical Ultraviolet-Visible Absorption Spectroscopy
163(52)
Experiment 6-1 Spectrophotometry in the Visible Region: Absorption Spectra, Beer's Law, and the Simultaneous Analysis of a Two-Component Mixture Supplementary Experiments:
168(13)
I Determination of a Mixture of Cobalt and Nickel
180(1)
II Determination of Chromium (as Cr(2)O(7)^2-) and Manganese (as MnO(4)^-) Mixtures
180(1)
III Simultaneous Determination of Fe(II) and Fe(III)
180(1)
Experiment 6-2 "Precision" Spectrophotometry Supplementary Experiments
181(6)
I Low-Absorbance Method
186(1)
II Ultimate Precision Method
187(1)
Experiment 6-3 Photometric End-Point Detection and Spectrophotometry in the Near-Infrared Region Supplementary Experiments:
187(6)
I Photometric Titration of a Mixture of p-Nitrophenol and m-Nitrophenol
192(1)
II Photometric Titration of Iron
193(1)
Experiment 6-4 The pK(a) of an Indicator Supplementary Experiments
193(5)
I The pK(a) of Other Indicators
197(1)
II The pK(a) of Methyl Orange: Simultaneous Analysis of Two Components in a Solution
197(1)
Experiment 6-5 Spectrophotometric Determination of Formulas and Stability Constants of Complex Ions Supplementary Experiments
198(9)
I Method of Continuous Variations: Determination of the Formula for an Iron(III)-Sulfosalicylate Complex
205(1)
II Mole-Ratio Method: Determination of the Formula for a Fe(II)-2.2'-Bipyridine Complex in Water
206(1)
III Slope-Ratio Method: Determination of the Formula of the Fe(II)-1,10-Phenanthroline Complex
207(1)
Experiment 6-6 Qualitative and Quantitative Analysis of Aromatic Hydrocarbon Mixtures
207(4)
Experiment 6-7 Analysis of Pharmaceutical Mixtures
211(1)
Experiment 6-8 Simultaneous Determination of Vitamin C and Vitamin E
212(3)
Chapter 7 / Absorption Spectroscopy of Electronic Transitions
215(7)
Experiment 7-1 Electronic Transitions in Organic Molecules
218(2)
Experiment 7-2 Electronic Transitions for Transition-Metal Complexes
220(2)
Chapter 8 / Infrared Spectroscopy
222(20)
Experiment 8-1 Infrared Spectrophotometry
227(9)
Experiment 8-2 Spectra of Aldehydes and Ketones
236(2)
Experiment 8-3 Determination of Monomers and Polymers
238(4)
Chapter 9 / Atomic Absorption and Atomic Emission Spectroscopy
242(24)
Experiment 9-1 Atomic Absorption Determinations
244(10)
Experiment 9-2 Determination of Mercury in Air, Water, and Fish by Flameless Atomic Absorption Spectrophotometry
254(4)
Experiment 9-3 Determination of Calcium, Iron, and Copper in Food by Atomic Absorption
258(2)
Experiment 9-4 Quantitative Determination of Alkali and Alkaline Earth Metals by Flame Photometry
260(5)
Supplementary Experiment: Determination of Sodium and Potassium in Cement
265(1)
Chapter 10 / Fluorescence Spectroscopy
266(20)
Experiment 10-1 Characterization of Quinine and its Determination
270(6)
Experiment 10-2 Determination of Fluorescein by Fluorometry
276(3)
Experiment 10-3 Determination of Pharmaceuticals (Acetylsalicylic and Salicylic Acids) by Fluorometry
279(4)
Experiment 10-4 Critical Micelle Concentration of Surfactants
283(1)
Experiment 10-5 Mercury(II) Determination by Oxidation of Thiamine to Thiochrome
284(2)
Chapter 11 / Nuclear Magnetic Resonance Spectroscopy
286(33)
Experiment 11-1 Proton NMR Spectra, Chemical Shifts, and Coupling Constants
293(2)
Experiment 11-2 pK(a) Values for Organic Bases
295(2)
Experiment 11-3 Proton NMR Spectrum of Acetylacetone: A Study of Keto-Enol Tautomerism
297(4)
Experiment 11-4 Determination of the Protonation Sequence of Methyliminodiacetic Acid and of the Stoichiometry of the Molybdenum-Methyliminodiacetic Complex by Proton NMR
301(1)
Experiment 11-5 Analysis of APC Tablets by Proton NMR
302(2)
Experiment 11-6 Determination of Amino Acid Structure and Sequence in Simple Dipeptides by Proton NMR
304(4)
Experiment 11-7 Magnetic Resonance Spectroscopy: Titration of Alanine Followed with NMR Detection
308(1)
Experiment 11-8 Magnetic Resonance Spectroscopy: Interpretations of (13)C NMR Spectra--A Study of Amygdalin ("Laetrile")
309(3)
Experiment 11-9 Magnetic Resonance Spectroscopy: ESR Spectra of Organic Free Radicals
312(5)
Experiment 11-10 Magnetic Resonance Spectroscopy: ESR Spectra of Transition-Metal Complexes
317(2)
Part 3 Separation Methods 319(84)
Chapter 12 / Gas Chromatography
321(23)
Experiment 12-1 Determination of Optimum Flow Rate in Gas Chromatography
328(5)
Experiment 12-2 Quantitative Analysis of Mixtures by Gas Chromatography
333(3)
Experiment 12-3 Resolution and Qualitative Identification of Hydrocarbons by Gas Chromatography
336(2)
Experiment 12-4 Study of a Consecutive Reaction: Kinetics and Gas Chromatography
338(3)
Experiment 12-5 Gas Phase Chromatography; Study of the Mechanism for an Elimination Reaction; Dehydration of Butanol
341(3)
Chapter 13 / High Performance Liquid Chromatography (HPLC)
344(17)
Experiment 13-1 Determination of Pharmaceuticals by High Performance Liquid Chromatography: Determination of Caffeine in Beverages
347(3)
Experiment 13-2 Separation of Urinary Compounds by High Performance Liquid Chromatography
350(3)
Experiment 13-3 Determination of Antibiotics by High Performance Liquid Chromatography
353(3)
Experiment 13-4 Separation of Aromatic Hydrocarbons by High Performance Liquid Chromatography
356(2)
Experiment 13-5 Separation of Carbohydrates by High Performance Liquid Chromatography
358(3)
Chapter 14 / Exclusion Chromatography
361(6)
Experiment 14-1 Exclusion Chromatography: Characterization of Hemoglobin
364(3)
Chapter 15 / Ion-Exchange Chromatography
367(13)
Experiment 15-1 Ion-Exchange Resins and Chelometric Titrations
369(5)
Experiment 15-2 Iron-Cobalt Separation by Ion Exchange
374(6)
Chapter 16 / Liquid-Solid Chromatography
380(7)
Experiment 16-1 Chromatographic Separation of cis and trans Azobenzenes Determined Spectrophotometrically
382(2)
Experiment 16-2 Quantitative Analysis of APC Tablets by Liquid-Solid Chromatography and Ultraviolet Spectroscopy
384(3)
Chapter 17 / Thin-Layer Chromatography (TLC)
387(9)
Experiment 17-1 Thin-Layer Chromatography and Separation of Amino Acid Derivatives
390(6)
Chapter 18 / Electrophoresis
396(7)
Experiment 18-1 Electrophoresis: Isoelectric Point of a Protein
400(3)
Appendices 403
Appendix 1 / Special Project Experiments from the Journal of Chemical Education, 1972-1982 405(5)
Appendix 2 / Reference Tables 410
Table A-1 Physical Constants and Units 410(1)
Table A-2 SI Derived Units 411(1)
Table A-3 Acidity Constants of Inorganic Substances 412(1)
Table A-4 Acidity Constants of Organic Substances 413(1)
Table A-5 Acid-Base Indicators 414(1)
Table A-6 Solubility-Product Constants 415(1)
Table A-7 Formation Constants (log K) of Some Metal Chelonates 416(3)
Table A-8 Formation Constants of Some Metal Complexes 419(1)
Table A-9 Standard and Formal Electrode Potentials at 25 degree C 420(4)
Table A-10 Potentials of the Common Reference Electrodes 424(1)
Table A-11 Equivalent Ionic Conductances at Infinite Dilution 424(1)
Table A-12 Polarographic Half-Wave Potentials 425(1)
Table A-13 Spectrophotometric Solvents for UV and IR Spectra 426(1)
Table A-14 Useful Spectral Regions for Absorption Cells and Instruments 426(1)
Table A-15 Emission Spectra; Principal Analysis Lines of the Elements 427

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