EXPERIMENTS IN PHYSICAL CHEMISTRY

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1 EXPERIMENTS IN PHYSICAL CHEMISTRY SIXTH EDITION DAVID P. SHOEMAKER CARL W. GARLAND JOSEPH W. NIBLER The Late Emeritus Professor of Chemistry Professor of Chemistry Professor of Chemistry Oregon State University Massachusetts Institute of Technology Oregon State University THE MCGRAW-HILL COMPANIES, INC. New York St. Louis San Francisco Auckland Bogota Caracas Lisbon London Madrid Mexico City Milan Montreal New Delhi San Juan Singapore Sydney Tokyo Toronto

2 Contents Preface I. INTRODUCTION Organization of the Book Preparation for an Experiment Execution of an Experiment Safety Recording of Experimental Data Literature Work Reports Sample Report Special Projects II. TREATMENT OF EXPERIMENTAL DATA 27 A. Caiculations and Presentation of Data Significant Figures Precision of Caiculations Analytical Methods Numerical Methods Graphs and Graphical Methods Exercises B. Uncertainties in Data and Results Errors Rejection of Discordant Data Statistical Treatment of Random Errors Significance Testing Propagation of Errors Case History of an Error Evaluation

3 Fundamental Limitations on Instrumental Precision 64 Summary 66 Exercises 68 III. USE OF COMPUTER SOFTWARE 71 Word Processors 71 Spreadsheets 72 Symbolic Mathematics Programs 82 Quantum Mechanical Programs 85 Exercises 88 IV. GASES Gas Thermometry Joule-Thomson Effect Heat-Capacity Ratios for Gases 105 V. TRANSPORT PROPERTIES OF GASES 117 Kinetic Theory of Transport Phenomena Viscosity of Gases Diffusion of Gases 134 VI. THERMOCHEMISTRY 145 Principles of Calorimetry Heats of Combustion Strain Energy of the Cyclopropane Ring Heats of Ionic Reaction 167 VII. SOLUTIONS Partial Molal Volume Cryoscopic Determination of Molecular Weight Freezing-Point Depression of Strong and Weak Electrolytes Chemical Equilibrium in Solution 193 VIII. PHASE EQUILIBRIA Vapor Pressure of a Pure Liquid Binary Liquid-Vapor Phase Diagram Binary Solid-Liquid Phase Diagram Liquid-Vapor Coexistence Curve and the Critical Point 222 IX. ELECTROCHEMISTRY Conductance of Solutions Temperature Dependence of EMF Activity Coefficients from Cell Measurements 241 X. CHEMICAL KINETICS Method of Initial Rates: Iodine Clock NMR Study of a Reversible Hydrolysis Reaction Enzyme Kinetics: Inversion of Sucrose 264

4 Contents VM 23. Kinetics of the Decomposition of Benzenediazonium Ion Gas-Phase Kinetics 280 XI. SURF ACE PHENOMENA Surface Tension of Solutions Physical Adsorption of Gases 300 XII. MACROMOLECULES Osmotic Pressure Intrinsic Viscosity: Chain Linkage in Polyvinyl Alcohol Helix-Coil Transition in Polypeptides 326 XIII. ELECTRIC AND MAGNETIC PROPERTIES Dipole Moment of Polar Molecules in Solution Dipole Moment of HCl Molecules in the Gas Phase Magnetic Susceptibility NMR Determination of Paramagnetic Susceptibility 369 XIV. SPECTROSCOPY Absorption Spectrum of a Conjugated Dye Infrared Spectroscopy: Vibrational Spectrum of S Raman Spectroscopy: Vibrational Spectrum of CC Vibrational-Rotational Spectra of HCl and DC Vibrational-Rotational Spectra of Acetylenes Band Spectrum of Nitrogen Absorption and Emission Spectra of Molecular Iodine Electron Spin Resonance Spectroscopy NMR Determination of Keto-Enol Equilibrium Constants NMR Study of Gas-Phase DCl-HBr Isotopic Exchange Reaction Solid-State Lasers: Radiative Properties of Ruby Crystals 462 XV. SOLIDS Determination of Crystal Structure by X-ray Diffraction Single-Crystal X-ray Diffraction with the Buerger Precession Camera Lattice Energy of Solid Argon Statistical Thermodynamics of Iodine Sublimation 514 XVI. COMPUTER INTERFACING 529 Computer Data Types 530 Hardware 533 Software 535 Computer Programming 538 Interfacing with Experiments 542 XVII. ELECTRONIC DEVICES AND MEASUREMENTS 554 Circuit Elements 554 Semiconductor Devices 558 Operational Amplifiers 566

5 VIII Contents Analog-to-Digital Conversion 571 Digital Multimeters 573 Potentiometer Circuits 575 Wheatstone Bridge Circuits 578 Capacitance Measurements 581 XVIII. TEMPERATURE 584 Temperature Scales 584 Triple-Point and Ice-Point Cell 588 Thermometers 589 Temperature Control 604 XIX. VACUUM TECHNIQUES 615 Introduction 615 Theoretical Background 615 Pumping Speed for a System 616 Desorption and Virtual Leaks 621 Pumps 622 Vacuum Gauges 630 Miscellaneous Vacuum Components 635 Design of Vacuum Lines 638 Leak Detection 640 Safety Considerations 642 XX. INSTRUMENTS 644 Balances 644 Barometers 648 Oscilloscopes 648 ph Meters 652 Polarimeters 654 Radiation Counters 656 Recorders, Plotters, and Printers 656 Refractometers 657 Signal-Averaging Devices 661 Spectroscopic Components 663 Spectroscopic Instruments 676 Timing Devices 683 XXI. MISCELLANEOUS PROCEDURES 685 Volumetrie Procedures 685 Purification Methods 690 Gas-Handling Procedures 691 Electrodes for Electrochemical Cells 697 Materials for Construction 698 Solders and Adhesives 704 Tubing Connections 706 Shopwork 708

6 XXII. LEAST-SQUARES FITTING PROCEDURES 710 Introduction 710 Foundations of Least Squares 711 Weights 716 Rejection of Discordant Data 718 Goodness of Fit 719 Comparison of Models 722 Uncertainties in the Parameters 725 Summary of Procedures 727 Sample Least-Squares Calculation 728 APPENDIXES 733 A. Glossary of Symbols 733 B. International System of Units and Concentration Units 736 C. Safety 739 D. Literature Work 746 E. Research Journals 753 F. Numerical Methods of Analysis 755 G. Barometer Corrections 764 Index 765 Endpapers Physical Constants and Conversion Factors Energy Conversion Table Relative Atomic Masses of the Elements front front back

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