Free download Analytical Chemistry for Technicians by John Kenkel

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John Kenkel

Table of Contents in Analytical Chemistry for Technicians by John Kenkel

1 Introduction to Analytical Science

1.1 Analytical Science Defined  

1.2 Classifications of  

1.3 The Sample  

1.4 The Analytical Strategy  

1.5 Analytical Technique and Skills  

1.6 The Laboratory Notebook  

1.7 Errors, Statistics, and Statistical Control  

1.7.1 Errors  

1.7.2 Elementary  

1.7.3 Normal  

1.7.4 Precision, Accuracy, and  

1.7.5 Statistical Control  

Experiments  

Experiment 1: Assuring the Quality of Weight  14

Experiment 2: Weight Uniformity of Dosing   

Questions and Problems  

2 Sampling and Sample Preparation

2.1 Introduction  

2.2 Obtaining the Sample   

2.3 Statistics of Sampling  

2.4 Sample  

2.4.1 Chain of Custody  

2.4.2 Maintaining Sample Integrity  

2.5 Sample Preparation: Solid  

2.5.1 Particle Size Reduction  

2.5.2 Sample Homogenization and  

2.5.3 Solid–Liquid  

2.5.4 Other Extractions from  

2.5.5 Total Dissolution  

2.5.6 Fusion  

2.6 Sample Preparation: Liquid Samples, Extracts, and Solutions of  28

2.6.1 Extraction from Liquid Solutions  

2.6.2 Dilution, Concentration, and Solvent Exchange  29

2.6.3 Sample  

Copyright © 2003 CRC Press, LLC

L1519_Frame_FM Page 16 Monday, November 3, 2003 11:26 AM

2.7 Reagents Used in Sample Preparation  

2.8 Labeling and Record  

Experiments  

Experiment 3: A Study of the Dissolving Properties of Water,

Some Common Organic Liquids, and Laboratory Acids  31

Questions and Problems  

3 Gravimetric Analysis

3.1 Introduction  

3.2 Weight vs.  

3.3 The Balance  

3.4 Calibration and Care of  

3.5 When to Use Which  

3.6 Details of Gravimetric  

3.6.1 Physical Separation Methods and Calculations  40

3.6.2 Chemical Alteration and Separation of the Analyte  48

3.6.3 Gravimetric  48

3.6.4 Using Gravimetric  

3.7 Experimental  

3.7.1 Weighing  

3.7.2 Weighing by Difference  

3.7.3 Isolating and Weighing Precipitates  

Experiments  

Experiment 4: Practice of Gravimetric Analysis Using Physical Separation  54

Experiment 5: The Percent of Water in Hydrated Barium Chloride  56

Experiment 6: The Gravimetric Determination of Sulfate in a Commercial  57

Experiment 7: The Gravimetric Determination of Iron in a Commercial Unknown

Questions and Problems  

4 Introduction to Titrimetric Analysis

4.1 Introduction  

4.2  

4.3 Review of Solution  

4.3.1 Molarity  

4.3.2 Normality  

4.4 Review of Solution Preparation  

4.4.1 Solid Solute and  

4.4.2 Solid Solute and Normality  

4.4.3 Solution Preparation by Dilution  

4.5 Stoichiometry of Titration  

4.6 Standardization  

4.6.1 Standardization Using a Standard Solution  73

4.6.2 Standardization Using a Primary  75

4.6.3 Titer  

4.7 Percent Analyte  

4.8 Volumetric Glassware  

4.8.1 The Volumetric  

4.8.2 The Pipet  

4.8.3 The  

4.8.4 Cleaning and Storing  

4.9 Pipetters, Automatic Titrators, and Other  88

4.9.1 Pipet  

4.9.2  

4.9.3 Bottle-Top Dispensers   

4.9.4 Digital Burets and Automatic  89

4.10 Calibration of Glassware and Devices  

4.11 Analytical Technique  

Experiments  

Experiment 8: Preparation and Standardization of HCl and NaOH Solutions  92

Experiment 9: Relationship of Glassware Selection to Variability of  93

Questions and Problems  

5 Applications of Titrimetric Analysis

5.1 Introduction  

5.2 Acid–Base Titrations and Titration  

5.2.1 Titration of Hydrochloric  

5.2.2 Titration of Weak Monoprotic Acids  

5.2.3 Titration of Monobasic Strong and Weak  101

5.2.4 Equivalence Point  

5.2.5 Titration of Polyprotic Acids: Sulfuric Acid and Phosphoric  103

5.2.6 Titration of Potassium  

5.2.7 Titration of Tris-(hydroxymethyl)amino  105

5.2.8 Titration of Sodium  

5.2.9 Alkalinity  

5.2.10 Back Titrations  

5.2.11 The Kjeldahl Method for  

5.2.12 Buffering Effects and Buffer  113

5.3 Complex Ion Formation  

5.3.1  

5.3.2 Complex Ion  

5.3.3 EDTA and Water  

5.3.4 Expressing Concentration Using Parts Per Million  123

5.3.5 Water Hardness  

5.4 Oxidation–Reduction Reactions  

5.4.1 Review of Basic Concepts and Terminology  127

5.4.2 The Ion-Electron Method for Balancing Equations  130

5.4.3 Analytical Calculations  

5.4.4 Applications  

5.5 Other  

Experiments  

Experiment 10: Titrimetric Analysis of a Commercial KHP Unknown for KHP  135

Experiment 11: Titrimetric Analysis of a Commercial Soda Ash Unknown

for Sodium Carbonate  

Experiment 12: Determination of Protein in Macaroni by the Kjeldahl  136

Experiment 13: Analysis of Antacid  

Experiment 14: Determination of Water Hardness  138

Questions and Problems   

6 Introduction to Instrumental Analysis

7 Introduction to Spectrochemical Methods

8 UV-VIS and IR Molecular Spectrometry

9 Atomic Spectroscopy

10 Other Spectroscopic Methods

11 Analytical Separations

12 Gas Chromatography

13 High-Performance Liquid Chromatography

14 Electroanalytical Methods

15 Physical Testing Methods

16 Bioanalysis

Appendix 1 Good Laboratory Practices

Appendix 2 Significant Figure

Appendix 3 Stoichiometric Basis for Gravimetric 495

Appendix 4 Solution and Titrimetric Analysis Calculation Formulas 497

Appendix 5 Answers to Questions and

Index

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