Basics of Analytical Chemistry and Chemical Equilibria E-Book

Brian M. Tissue

• Herausgeber: John Wiley & Sons
• Kategorie: Wissenschaft und neue Technologien
• Sprache: Englisch

Seitenzahl: 847

Veröffentlichungsjahr: 2023

Beschreibung

BASICS OF ANALYTICAL CHEMISTRY AND CHEMICAL EQUILIBRIA

Familiarize yourself with the fundamentals of analytical chemistry with this easy-to-follow textbook

Analytical chemistry is the study of chemical composition, concerned with analyzing materials to discover their constituent substances, the amounts in which these substances are present, and more. Since materials exist in different states and undergo reactions, analytical chemistry is also concerned with chemical equilibria, the state at which various reactants and substances will undergo no observable chemical change without outside stimulus. This field has an immense range of practical applications in both industry and research and is a highly desirable area of expertise for the next generation of chemists.

Basics of Analytical Chemistry and Chemical Equilibria provides an introduction to this foundational subject, ideal for specialized courses. It introduces not only the core concepts of analytical chemistry but cultivates mastery of various instrumental methods by which students and researchers can undertake their own analyses. Now updated to include the latest research and expanded coverage, Basics of Analytical Chemistry and Chemical Equilibria promises to situate a new generation of readers in this growing field.

Readers of the second edition of Basics of Analytical Chemistry and Chemical Equilibria will also find:

• A new chapter on structure determination
• Revised and expanded descriptions of chemical instrumentation
• ‘You-try-it’ exercises throughout to further develop practical student knowledge
• Compannion website of associated materials including end-of-chapter solutions, spreadsheets for student use, and more

Basics of Analytical Chemistry and Chemical Equilibria is an ideal textbook for students in chemistry, biochemistry, and environmental science, as well as students in related fields, including chemical engineering and materials science, for whom analytical chemistry offers a useful toolset.

Leseprobe

BASICS OF ANALYTICAL CHEMISTRY AND CHEMICAL EQUILIBRIA: A QUANTITATIVE APPROACH

By

BRIAN M. TISSUE

Virginia TechDepartment of ChemistryBlacksburg, VA

Second Edition

Copyright © 2023 by John Wiley & Sons, Inc. All rights reserved.

Published by John Wiley & Sons, Inc., Hoboken, New Jersey.

Published simultaneously in Canada.

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Cover Images: Background: © kundoy/Getty Images; Figure: Courtesy of Brian M. Tissue

Cover Design: Wiley

Set in 11/13pt TimesNewRomanPSMT by Integra Software Services Pvt. Ltd, Pondicherry, India

Contents

Cover

Title page

Copyright

PREFACE

ABOUT THE COMPANION WEBSITE

I QUANTITATIVE ANALYSIS USING REACTIONS THAT GO TO “COMPLETION”

1 MAKING MEASUREMENTS

1.1 Introduction

1.2 Glp and a Few Other Important Acronyms

1.3 Precision and Random Error

1.4 Discarding a Suspected Outlier

1.5 Calibration

1.6 Maintaining Accurate Results

Practice Exercises

2 SAMPLE PREPARATION, EXTRACTIONS, AND CHROMATOGRAPHY

2.1 Sampling and Control Samples

2.2 Sample Preparation

2.3 Solvents and Solutions

2.4 Introduction to Solubility

2.5 Extraction and Partitioning Theory

2.6 Introduction to Stationary Phases

2.7 Solid-Phase Extraction (SPE)

2.8 Column Chromatography

Practice Exercises

3 CLASSICAL METHODS

3.1 Introduction

3.2 Review of Chemical Reactions

3.3 Reactions in Aqueous Solution

3.4 Gravimetry

3.5 Titration

3.6 Titration Curves

3.7 Coulometry

Practice Exercises

4 MOLECULAR SPECTROSCOPY

4.1 Introduction

4.2 Properties of EM Radiation

4.3 Electromagnetic Spectrum

4.4 Spectroscopic Transitions

4.5 UV/Vis Absorption Spectroscopy

4.6 UV/Vis Instrumentation

4.7 Beer–Lambert Law

4.8 Molecular Fluorescence

Practice Exercises

II REACTIONS THAT DO NOT GO TO “COMPLETION.” EQUILIBRIA IN AQUEOUS SOLUTIONS

5 ACID–BASE EQUILIBRIA AND ACTIVITY

5.1 Acids and Bases

5.2 Weak Acids and Weak Bases

5.3 Water and Kw

5.4 Acid Strength

5.5 The Concept of Activity

5.6 Acid–Base Equilibrium Calculations

Practice Exercises

6 BUFFER SOLUTIONS AND POLYPROTIC ACIDS

6.1 Buffer Solutions

6.2 Alpha Fraction Plots

6.3 Weak Acid Titration Curve

6.4 Polyprotic Acids

Practice Exercises

7 METAL–LIGAND COMPLEXATION

7.1 Complex Terminology

7.2 Complex Equilibria

7.3 Competing Equilibria

7.4 Stepwise Complexation

7.5 Immunoassays

Practice Exercises

8 PRECIPITATION EQUILIBRIA

8.1 Precipitate Equilibrium

8.2 Molar Solubility

8.3 Common-Ion Effect

8.4 Precipitation and Competing Equilibria

8.5 Drinking Water

Practice Exercises

III INSTRUMENTAL METHODS AND ANALYTICAL SEPARATIONS

9 ELECTROANALYTICAL CHEMISTRY

9.1 Introduction

9.2 Standard Reduction Potentials

9.3 Using Half Reactions

9.4 Background on Spontaneous Reactions and Equilibrium

9.5 Reaction Energies, Voltages, and the Nernst Equation

9.6 Electrochemical Cells

9.7 Potentiometry

9.8 Ion-Selective Electrodes (ISE)

9.9 Voltammetry

Practice Exercises

10 ATOMIC SPECTROMETRY

10.1 Atomization

10.2 Atomic Absorption Spectrometry (AAS)

10.3 Atomic Emission Spectrometry (AES)

10.4 Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

10.5 Other Mass Spectrometer Designs

Practice Exercises

11 MOLECULAR STRUCTURE DETERMINATION

11.1 Introduction

11.2 Molecular Mass Spectrometry

11.3 Fourier-Transform Infrared Spectroscopy

11.4 FTIR Instrumentation

11.5 Nuclear Magnetic Resonance Spectroscopy

11.6 NMR Instrumentation

Practice Exercises

12 ANALYTICAL SEPARATIONS

12.1 Thin-Layer Chromatography

12.2 Chromatogram Terminology

12.3 Separation Efficiency

12.4 Gas Chromatography (GC)

12.5 Gas Chromatography Mass Spectrometry (GC-MS)

12.6 High Performance Liquid Chromatography

12.7 Electrophoresis

Practice Exercises

INDEX

End User License Agreement

List of Tables

CHAPTER 01

TABLE 1.1 Measurement Terms

TABLE 1.2 Measurement Strategies

TABLE 1.3 SI Base Units

TABLE 1.4 Common Numerical Prefixes

TABLE 1.5 SI Derived Units

TABLE 1.6 Common Concentration Units

TABLE 1.7 Titration Results

TABLE 1.8 Table of Critical...

TABLE 1.9 Critical Values...

TABLE 1.10 Values of

R

for...

TABLE 1.11 Riboflavin Spectral Data

TABLE 1.12 Examples of Primary Standards

TABLE 1.13 Examples of Reference Materials

CHAPTER 02

TABLE 2.1 Sampling Plans

TABLE 2.2 Control Samples

TABLE 2.3 Error Sources in...

TABLE 2.4 NIST SRMs for Lead Analysis

TABLE 2.5 Sample Preparation Methods

TABLE 2.6 Definitions for...

TABLE 2.7 Names of Organic...

TABLE 2.8 Relative Polarity...

TABLE 2.9 Polarity Index...

TABLE 2.10 Solubility of...

TABLE 2.11 Solubility Rules

TABLE 2.12 Aqueous Solubility...

TABLE 2.13 Counterions of Strong...

TABLE 2.14 Methods of Analyte...

TABLE 2.15 Octanol–Water...

TABLE 2.16 Types of Stationary...

TABLE 2.17 Adsorption and...

TABLE 2.18 Ion exchange...

CHAPTER 03

TABLE 3.1 Reaction Types...

TABLE 3.2 Simplified Precipitation...

TABLE 3.3 Precipitating Agents...

TABLE 3.4 Acid–Base Indicators...

TABLE 3.5 Indicators for Other Types...

TABLE 3.6

Β

1

Values...

CHAPTER 04

TABLE 4.1 Refractive...

TABLE 4.2 Classification...

TABLE 4.3 Common Prefixes...

TABLE 4.4 Types of Electronic...

TABLE 4.5 Onset of UV Absorption...

TABLE 4.6 Attenuation of Photons...

TABLE 4.7 Relationship Between...

TABLE 4.8 Effect of Stray Light...

TABLE 4.9 Sample Absorbance Data

TABLE 4.10 Light Transmittance...

CHAPTER 05

TABLE 5.1 Pauling Electronegativities

TABLE 5.2 Common Strong Acids...

TABLE 5.3 Checking Charge...

TABLE 5.7

K

a

Values...

TABLE 5.8

K

a

Values...

TABLE 5.4 Conductivity of Water

TABLE 5.5

K

w

Versus...

TABLE 5.6 Relative Strength of Selected...

TABLE 5.9 Ion Size Parameter for Cations...

TABLE 5.10 Ion Size Parameter for Anions...

TABLE 5.11 Activity Coefficients...

CHAPTER 07

TABLE 7.1 Examples of Oxyanions

TABLE 7.2

β

Values...

TABLE 7.3 Acidity due to Metal...

TABLE 7.4 Predicted Optimal pH...

TABLE 7.5 Selected Stepwise...

CHAPTER 08

TABLE 8.1

K

sp

Values...

TABLE 8.2 Calculated Values...

TABLE 8.3 Calculated and Measured...

CHAPTER 09

TABLE 9.1 Common Redox Processes

TABLE 9.2 Common Oxidation...

TABLE 9.3 Relative Strength...

TABLE 9.4

E

° Values for...

CHAPTER 10

TABLE 10.1 Temperature of Different...

TABLE 10.2 Relative Strength of...

TABLE 10.3 Examples of Isobaric...

TABLE 10.4 Characteristics of...

TABLE 10.5 Common Mass Analyzer...

CHAPTER 11

TABLE 11.1 Summary of Structure...

TABLE 11.2 Spectral Range...

TABLE 11.3 Common Molecular...

TABLE 11.4 Exact Mass and...

TABLE 11.5 Trends in Energy...

TABLE 11.6 IR Absorption Bands...

TABLE 11.7 Chemical Shifts...

CHAPTER 12

TABLE 12.1 Common TLC Mobile...

TABLE 12.2 Internal Diameter...

TABLE 12.3 GC Stationary Phases

TABLE 12.4 Types of Stationary...

TABLE 12.5 HPLC Detectors

TABLE 12.6 LC-MS Ionization Methods

TABLE 12.7 Chromatogram Peaks...

TABLE 12.8 Chromatogram Peaks...

List of Illustrations

CHAPTER 01

Figure 1.1 The results from...

Figure 1.2 Results of four...

Figure 1.3 Histogram and normal distribution.

Figure 1.4 Source of a systematic error.

Figure 1.5 (a) One-point...

Figure 1.6 Linear range...

Figure 1.7 Absorbance spectra...

Figure 1.8 Example of a...

Figure 1.9 Plot illustrating...

Figure 1.10 Analytical balance.

Figure 1.11 Volumetric glassware.

CHAPTER 02

Figure 2.1 Map of a stratified...

Figure 2.2 Example of a control chart.

Figure 2.3 Abbreviated sample...

Figure 2.4 A combination...

Figure 2.5 Illustration...

Figure 2.6 A crown ether...

Figure 2.7 Schematic of a solid...

Figure 2.8 SPE cartridge...

Figure 2.9 Microscopic...

Figure 2.10 (a) Methylphenidate...

Figure 2.11 Schematic of a column...

Figure 2.12 Microscopic schematic...

CHAPTER 03

Figure 3.1 Reactants A and B...

Figure 3.2 Schematic of solution...

Figure 3.3 Titration with...

Figure 3.4 Metal–EDTA complex.

Figure 3.5 Calmagite indicator...

Figure 3.6 Titration curve...

Figure 3.7 Concentration dependence...

Figure 3.8 Gran plot of titration curve.

Figure 3.9 Schematic of...

CHAPTER 04

Figure 4.1 EM radiation traveling...

Figure 4.2 Regions of the...

Figure 4.3 Visible or IR light...

Figure 4.4 Promotion to an...

Figure 4.5 The solar spectrum.

Figure 4.6 Allowed energies...

Figure 4.7 Hg emission spectrum.

Figure 4.8 Ground and excited...

Figure 4.9 Relative energies...

Figure 4.10 UV/Vis absorption...

Figure 4.11 Schematic of a visual...

Figure 4.12 Schematic of a simple...

Figure 4.13 Schematic of a grating...

Figure 4.14 Schematic of an optical...

Figure 4.15 Light power measurements...

Figure 4.16 Light power as a function...

Figure 4.17 Top-view schematic...

Figure 4.18 Plot of absorbance...

Figure 4.19 Tartrate ligand.

Figure 4.20 Calibration curve...

Figure 4.21 Molecular energy-level...

Figure 4.22 Excitation and...

Figure 4.23 Schematic of a simple...

CHAPTER 05

Figure 5.2 Examples of structures...

Figure 5.1 Examples of structures...

Figure 5.3 Diffusion driving...

Figure 5.4 Diffusion driving...

Figure 5.5 Steps before setting...

CHAPTER 06

Figure 6.1 Alpha plot...

Figure 6.2 Titration curves...

Figure 6.3 Concentration...

Figure 6.4 Structures of...

Figure 6.5 Alpha fraction...

Figure 6.6 Alpha plots for...

Figure 6.7 Alpha plots for...

CHAPTER 07

Figure 7.1 Examples of...

Figure 7.2 Alpha plots...

Figure 7.3 Calmagite indicator...

Figure 7.4 Alpha plots to...

Figure 7.5 Alpha plots for...

Figure 7.6 Log(alpha) plots...

Figure 7.7 Steps in an...

Figure 7.8 Schematic...

CHAPTER 08

Figure 8.1 Equilibrium...

CHAPTER 09

Figure 9.1 Chlorine oxidation...

Figure 9.2 Reaction coordinate...

Figure 9.3 Reaction coordinate...

Figure 9.4 Schematic of an...

Figure 9.5 Two containers...

Figure 9.6 An electrochemical...

Figure 9.7 Voltage measurement...

Figure 9.8 Set up to make...

Figure 9.9 An integrated...

Figure 9.10 ISFET schematic...

Figure 9.11 Simplified...

Figure 9.12 Schematic of...

Figure 9.13 Linear sweep.

Figure 9.14 Normal pulse...

Figure 9.15 Differential...

Figure 9.16 Cyclic voltammogram.

CHAPTER 10

Figure 10.1 Atomization process...

Figure 10.2 Schematics of (a) cross-flow...

Figure 10.3 Schematic of pulsed...

Figure 10.4 Schematic of laser...

Figure 10.5 Schematic of an atomic...

Figure 10.6 Schematic of a flame...

Figure 10.7 Flame AAS calibration...

Figure 10.8 Sequence of steps...

Figure 10.9 Schematic of a cold-vapor...

Figure 10.10 Schematic of an ICP...

Figure 10.11 Schematic of an atomic...

Figure 10.12 Resolution of adjacent...

Figure 10.13 Schematic of a polychromator.

Figure 10.14 Schematic of mass...

Figure 10.15 Schematic of a quadrupole...

Figure 10.16 Mass filtering by the...

Figure 10.17 Summary of atomic...

Figure 10.18 Cut-through schematic...

Figure 10.19 Top-down schematic...

Figure 10.20 Schematic of a reflectron...

Figure 10.21 Example of a TOF mass...

CHAPTER 11

Figure 11.1 Electron-ionization mass...

Figure 11.2 Accurate mass resolution...

Figure 11.3 Vibrational levels...

Figure 11.4 IR absorption spectrum...

Figure 11.5 Schematic of an FTIR...

Figure 11.6 Schematic of an attenuated...

Figure 11.7 Splitting of nuclear...

Figure 11.8 NMR spectrum...

Figure 11.9 NMR spectrum...

Figure 11.10 Side-view schematic...

Figure 11.11 Free-induction decay...

CHAPTER 12

Figure 12.1 Spotting a TLC plate...

Figure 12.2 Separation of sample...

Figure 12.3 Visualized spots...

Figure 12.4 Chromatogram...

Figure 12.5 (a) Reference...

Figure 12.6 Plate height...

Figure 12.7 Schematic of a gas...

Figure 12.8 Schematic of mass...

Figure 12.9 Total-ion (bottom)...

Figure 12.10 Schematic...

Figure 12.11 Structures...

Figure 12.12 HPLC chromatogram...

Figure 12.13 Schematic of a gel...

Figure 12.14 Schematic...

Figure 12.15 Schematic...

Figure 12.16 Schematic...

Guide

Cover

Title page

Copyright

Table of Contents

PREFACE

ABOUT THE COMPANION WEBSITE

Begin Reading

INDEX

End User License Agreement

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PREFACE

This text will introduce you to analytical chemistry: the science of making quantitative measurements. Quantifying the individual components in a complex sample is an exercise in problem solving. An effective and efficient analyst will have expertise in

sampling, sample processing, and method validation;

the chemistry that can occur in a sample before and during analysis;

selecting an appropriate analytical method; and

proper record keeping, data analysis, and reporting of results.

I do not attempt to be comprehensive in this text. Samples that require analysis are so diverse that it is not possible to describe every sample preparation protocol, separation method, and measurement technique. These details are contained in handbooks and method compilations, many of which are now accessible from online sources. This text emphasizes the fundamental chemical and physical concepts that underlie the analytical methods. With an understanding of the fundamental concepts, a scientist faced with a difficult analysis can apply the most appropriate techniques, identify when a particular problem cannot be solved with existing methods, and develop new analytical methods. The proficient analyst will also be alert to interferences and problems in analytical measurements and recognize when an “answer” might not be correct.

I organize the discussion of the core principles of analytical chemistry into three parts:

Part I: Analytical concepts such as calibration and uncertainty, sample preparation, classical (wet-chemical) methods, and molecular UV/Vis spectroscopy

Part II: Chemical equilibria involving acids, bases, complexes, and insoluble precipitates

Part III: Electroanalytical methods, atomic spectrometry, molecular structure determination, and chromatographic separations

The analytical methods in Part I rely on reactions that go to completion. Part II is a detailed treatment of chemical equilibria—reactions in which reactants and products coexist. Chemical equilibria are critical to many aspects of chemical, biochemical, and environmental systems. Part III describes the most common instrumental methods of analysis, illustrating many of the tools of the trade for making quantitative measurements. Even if your future career veers away from science, you will find the problem-solving and graphical data analysis skills developed in this text to be useful.

Many of the topics in this text follow directly from first-year college chemistry. You will want access to a general chemistry text or online resource to refresh your memory of the underlying principles of physical processes and chemical species. The level of this text presumes that you know

Basic math

Algebra

Exponential functions

Calculating and plotting in a spreadsheet

Basic chemistry

Predicting properties based on the periodic table

The nature of chemical compounds

Stoichiometry and balancing reactions

Reaction types

Acid–base

Complexation

Precipitation

Reduction and oxidation (redox)

The beginning of each chapter lists learning outcomes that serve as a brief outline to help categorize new material. After completing a chapter, make a concept map to help yourself see the big picture and underlying concepts. You will often encounter a repeat of concepts in the text. Making connections with prior material makes learning analytical concepts much easier. Treating every topic as something new becomes overwhelming. Each chapter contains sample calculations and practice exercises. I assume that your goal is success. Achieving success requires skills, and acquiring skills takes practice.

Variables and constants are italicized to not be confused with other text. As much as possible, I use the conventions and terminology in the IUPAC Gold Book.1 You will find other symbols in other books and resources, so use the context to decipher the differences. This second edition adds substantial information on instrumental methods and manufacturers will often use different terms for similar instruments. Relevant spreadsheets and links to useful resources are available at https://www.achem.org.

BRIAN M. TISSUEAugust 2022

Blacksburg, VA

Notes

1

See

IUPAC Compendium of Chemical Terminology

, “The Gold Book,”

https://goldbook.iupac.org

; Accessed August 2022.

ABOUT THE COMPANION WEBSITE

This book is accompanied by a companion website:

www.wiley.com/go/tissue/analyticalchemistry2e

This website includes:

Solutions to the end-of-chapter practice exercises.

Spreadsheet templates and solution guides for the “You-Try-It” exercises.

A glossary of analytical chemistry terms.

General spreadsheets for common analytical calculations.

PART I QUANTITATIVE ANALYSIS USING REACTIONS THAT GO TO “COMPLETION”